Datasets:

sofc_materials_articles

like 7

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[ "Fabrication of low-temperature solid oxide fuel cells with a nanothin protective layer by atomic layer deposition Fabrication of low-temperature solid oxide fuel cells with a nanothin protective layer by atomic layer deposition JiSanghoon1ChangIkwhang1LeeYoon Ho2ParkJoonho2PaekJun Yeol2LeeMin Hwan3ChaSuk Won2 1Graduate School of Convergence Science and Technology, Seoul National University, 864-1 Lui Dong, Yeongtong-Gu, Suwon, Gyeonggi-Do, 433-270, South Korea 2School of Mechanical and Aerospace Engineering, Seoul National University, 599 Gwanak-ro, Gwanak-gu, Seoul, 151-742, South Korea 3School of Engineering, University of California, Merced, 5200 North Lake Road, Merced, CA, 95343, USA Anode aluminum oxide-supported thin-film fuel cells having a sub-500-nm-thick bilayered electrolyte comprising a gadolinium-doped ceria (GDC) layer and an yttria-stabilized zirconia (YSZ) layer were fabricated and electrochemically characterized in order to investigate the effect of the YSZ protective layer.", "The highly dense and thin YSZ layer acted as a blockage against electron and oxygen permeation between the anode and GDC electrolyte.", "Dense GDC and YSZ thin films were fabricated using radio frequency sputtering and atomic layer deposition techniques, respectively.", "The resulting bilayered thin-film fuel cell generated a significantly higher open circuit voltage of approximately 1.07 V compared with a thin-film fuel cell with a single-layered GDC electrolyte (approximately 0.3 V).", "Atomic layer deposition Protective layer Thin-film solid oxide fuel cell Yttria-stabilized zirconia Gadolinium-doped ceria Anodic aluminum oxide Background Solid oxide fuel cells (SOFCs) normally operate at considerably high temperatures (>700°C) to facilitate ionic charge transport and electrode kinetics [1,2].", "Encountered by issues such as limited material selection and poor cell durability, many researchers have tried to reduce the operating temperature [3-5].", "However, lower operating temperature led to a significant sacrifice in energy conversion efficiency due to the resulting increase in ohmic and activation losses [1].", "There are roughly two ways to minimize the ohmic loss surging at lower operating temperatures.", "One is to reduce the thickness of the electrolyte, and the other is to synthesize materials with higher ionic conductivities.", "First, the strategy to reduce in electrolyte thickness has been carried out by many research groups [6-10].", "Shim et al. demonstrated that a fuel cell employing a 40-nm-thick yttria-stabilized zirconia (YSZ) can generate a power density of 270 mW/cm2 at 350°C [11], while Kerman et al. demonstrated 1,037 mW/cm2 at 500°C from a 100-nm-thick YSZ-based fuel cell [12].", "Another approach of minimizing ohmic loss is using electrolytes with higher ionic conductivities.", "Gadolinium-doped ceria (GDC) has been considered as a promising electrolyte material due to its excellent oxygen ion conductivity at low temperatures [13,14].", "However, the tendency of GDC being easily reduced at low oxygen partial pressures makes its usage as a fuel-cell electrolyte less attractive because the material will have a higher electronic conductivity as it is reduced.", "For this reason, many studies have been performed to prevent electronic conduction through GDC film by placing an electron-blocking layer in the series [15-17].", "Liu et al. demonstrated the electron-blocking effect of a 3-μm-thick YSZ layer in a thin-film fuel cell with a GDC/YSZ bilayered electrolyte [18].", "If the GDC electrolyte thickness was reduced down to a few microns, another problem emerges, i.e., oxygen gas from the cathode side starts to permeate through the thin GDC electrolyte [13,19].", "For the reasons mentioned, the application of a protective layer is essential for GDC-based thin-film fuel cells.", "Recently, Myung et al. demonstrated that a thin-film fuel cell having a 100-nm-thick YSZ layer deposited by pulsed laser deposition onto a 1.4-μm-thick GDC layer actually prevented both the reduction of ceria at low oxygen partial pressures and oxygen permeation across the GDC thin layer [20].", "For the development of large-scale thin-film fuel cells, an anodic aluminum oxide (AAO) template has been considered as their substrate due to its high scalability potential.", "However, commercially available AAO templates have a considerably rough surface unlike silicon-based substrates, which have been used for conventional thin-film fuel cells.", "For this reason, atomic layer deposition (ALD) technique was employed to deposit a highly conformal and dense YSZ layer to minimize uncontrolled pinholes and/or morphological irregularities.", "In this report, we demonstrate a prototypical, AAO-supported thin-film fuel cell with a bilayered electrolyte comprising a GDC film and a thin protective YSZ layer.", "The radio frequency (RF)-sputtered GDC layer with excellent oxygen ion conductivity is used as the primary electrolyte layer, while the YSZ layer deposited by ALD technique prevents the reduction of ceria at low oxygen partial pressure and oxygen permeation across the GDC thin layer.", "To investigate the effect of ALD YSZ layer as a protective layer, the electrochemical performance of a GDC/YSZ bilayered thin-film electrolyte fuel cell is compared with that of a single-layered GDC-based thin-film fuel cell.", "Methods Thin-film characterization Chemical composition of thin films was analyzed by X-ray photoelectron spectroscopy (XPS) (AXIS Hsi, Kratos Analytical, Ltd., Manchester, UK).", "Possible surface contamination was eliminated by 150 eV of Ar-ion etching for 30 s prior to XPS analysis.", "The microstructure of thin films was investigated using focused ion beam and field emission scanning electron microscopy (FE-SEM) (Quanta 3D FEG, FEI Company, Hillsboro, OR, USA), and a few nanometer-thick Pt layer was coated on samples to prevent thin films from being etched by FE-SEM imaging.", "Electrochemical evaluation A test cell was attached to a custom-made hydrogen feeding chamber using a ceramic adhesive (CP4010, Aremco Products, Inc., Briarcliff Manor, NY, USA) and heated to 450°C using a halogen heating system.", "Dry H2 gas with a mass flow of 25 sccm was supplied to the anode side, and cathode was exposed to atmospheric environment.", "Anode was connected to a silver wire, and cathode was contacted by a hardened steel probe.", "Polarization of thin-film fuel cells was analyzed using an electrochemical testing system (1287/1260, Solartron Analytical, Hampshire, UK).", "Results and discussion Thin-film electrolyte fabrication GDC thin-film was fabricated by a commercial sputter (A-Tech System Ltd., Incheon, South Korea).", "Gd-Ce alloy (with 10 at.% Gd) was used as the GDC target.", "Target-to-substrate (T-S) distance was 80 mm.", "GDC thin films were deposited at a mixed Ar/O2 gas pressure of 5 mTorr.", "Volume fraction of O2 to Ar was 0.2.", "RF power was set at 150 W.", "The growth rates of GDC thin films deposited at 100°C and 500°C were approximately 42 and 20 nm/h, respectively.", "Considering that the packing density of GDC thin-film increases as the substrate temperature increases [21], the substrate was heated to a high temperature of 500°C [1] in order to accommodate more volume for bulk ionic conduction.", "To determine the chemical composition of GDC thin films, XPS analysis was carried out.", "A GDC thin-film deposited at 500°C (GDC-H) was compared to a film prepared at room temperature (GDC-R).", "Figure 1a,b respectively shows the XPS spectra of Ce 3d and Gd 4d core levels of GDC-R and GDC-H.", "As shown in Figure 1a, the Ce 3d core level of GDC-R did not show spin orbital doublets (V′, U′) unlike GDC-H, which is a characteristic of the Ce3+ binding state [22].", "This result reveals that GDC-H contains reduced cerium oxide (e.g., Ce2O3) as well as cerium dioxide.", "The Gd 4d core level in Figure 1b illustrated characteristic peaks that are very similar to those of gadolinium oxide, and there was no distinct difference between the two samples.", "As for atomic concentrations, GDC-H had a higher Gd doping concentration (Gd 4d ≈ 13%) than the GDC target (approximately 10%).", "It is tentatively attributed to the fact that cerium oxide with a lower molecular weight becomes more volatile than gadolinium oxide as substrate temperature increases [23].", "Figure 1 XPS spectra of (a) Ce 3d and (b) Gd 4d core levels of GDC thin films.", "We applied the ALD technique, thus enabling excellent step coverage to fabricate the ultrathin conformal YSZ layer using a commercial ALD system (Plus-100, Quros Co., Ltd., Osan, South Korea) [24,25].", "Prior to the deposition of a YSZ thin-film, zirconia and yttria films were separately deposited and characterized for a systematic study.", "Both films were fabricated by repeating the sequence of precursor pulse (3 s), purge (20 s), oxidant pulse (1 s), and purge (10 s).", "Tetrakis(dimethylamido)zirconium, Zr(NMe2)4, and Tris(methylcyclopentadienyl)yttrium, Y(MeCp)3, were used as precursors for zirconium and yttrium, respectively.", "The precursor was delivered using an electropolished stainless steel bubbler fed by Ar gas with 99.99% purity.", "O2 gas was used as the oxidant, and stage temperature was set to 250°C.", "The temperatures of canisters with charged precursors were 40°C and 180°C, and the line temperatures were 60°C and 210°C for zirconia and yttria deposition, respectively.", "The growth rates of both zirconia and yttria films during the initial 1,000 cycles were approximately 1 Å/cycle.", "Although these growth rates were somewhat lower than the reported values (1.2 to 1.5 Å/cycle) [11], the film thickness increased proportionally with the deposition cycles.", "XPS analyses were performed to determine the chemical composition of an approximately 100-nm-thick zirconia film and an approximately 100-nm-thick yttria film.", "The atomic concentrations in the zirconia thin-film were as follows: for Zr 3d, it was 41.6%, and for O 1s, it was 58.4%; they were somewhat different from the expected stoichiometry of ZrO2.", "It is attributed to the fact that reduced zirconium (e.g., Zr0 3d5/2 or Zr2+ 3d5/2) was partially combined with O2 during the ALD process, as indicated in the curve fitting result of Figure 2a [26].", "The atomic concentrations of the yttria thin-film were Y 3d = 40.9% and O 1s = 59.1%, which are well aligned with the stoichiometry of Y2O3.", "The Y 3d5/2 peak was located at a binding energy of 156.7 eV, as shown in Figure 2b [27].", "Figure 2 XPS spectra of (a) Zr 3d and (b) Y 3d core levels of zirconia/yttria thin films.", "Subsequently, YSZ thin films were fabricated by co-deposition of zirconia and yttria.", "Zirconia was deposited prior to yttria deposition.", "Yttria mole fraction in the ALD YSZ thin-film was controlled by changing the ratio of deposition cycles for zirconia and yttria.", "The yttria mole fraction is widely known to determine oxygen ion conductivity in the YSZ, and 8% mole yttria was reported to render the maximum oxygen ion conductivity [1].", "When the ratio of zirconia and yttria ALD cycle was 7:1, the atomic concentrations of the YSZ thin-film were as follows: Zr 3d = 24.2%, Y 3d = 3.6%, and O 1s = 72.1%, which were also determined by an XPS analysis.", "The Y2O3 mole fraction, x, in the YSZ chemical formula of (ZrO2)1−x(Y2O3)x was approximately 0.07.", "In the case of the YSZ thin-film, the XPS spectra corresponding to an under-stoichiometric ZrO2 did not appear, unlike those in the zirconia thin-film.", "Design of AAO-supported GDC/YSZ bilayered thin-film fuel cell A commercial AAO (Synkera Technology Inc., Longmont, CO, USA) template with an 80-nm pore and a 100-μm height was used as the substrate to leverage their high density of nanopores and resulting electrochemical reaction sites [28,29].", "Pt electrode was fabricated by a commercial sputter (A-Tech System Ltd.).", "Pt with 99.9% purity was used as the Pt target, and the T-S distance was 100 mm.", "The deposition was conducted at room temperature, and the direct current power was set to 200 W.", "The Pt anode was deposited on the AAO template in an area of 10 × 10 mm2.", "Dense Pt anodes were deposited at a 5-mTorr Ar pressure, having the growth rate of approximately 60 nm/min.", "Subsequently, YSZ and GDC electrolytes with an area of 9 × 9 mm2 were deposited on the Pt anode.", "The critical thickness ratio of the YSZ layer to the GDC layer to prevent the reduction of ceria, which was determined considering the distribution of oxygen activity through the thickness of a bilayer, was reported to be approximately 10−4 at 800°C and was expected to decrease further at lower temperatures [30].", "For this reason, the required minimum thickness of the YSZ layer for electron blockage, if the thickness of GDC layer is 420 nm, is only approximately 0.4 Å.", "However, a much thicker YSZ film (40 nm) was deposited on the anode side to compensate the rough morphological variations of the Pt-coated AAO surface.", "The GDC layer, which was 420-nm thick, was then deposited on the YSZ layer.", "Oxygen reduction reaction happening at the cathode is widely known to cause a significantly greater activation loss compared with the hydrogen oxidation reaction occurring at the anode [1].", "In order to facilitate cathode reaction, a porous Pt cathode was prepared by depositing at a much higher Ar pressure of 90 mTorr than that used for anode deposition (5 mTorr Ar).", "The cathode thickness was approximately 200 nm.", "The growth rate still remained at approximately 60 nm/min.", "The Pt cathode, which effectively determines the nominal area of active cell, was deposited using a mask with 1 × 1 mm2 openings.", "Electrochemical evaluation of thin-film fuel cells Thin-film fuel cells with 850-nm-thick GDC and 850-nm-thick Sn0.9In0.1P2O7 (SIPO) electrolytes were fabricated to study further how the ALD YSZ layer have the influence on electrochemical performance [31].", "Except for the electrolyte, other cell components were equal to those for GDC/YSZ bilayered thin-film fuel cell.", "For a comparison with GDC-based cells (cell 1, Pt/GDC/Pt), we fabricated SIPO-based cells (cell 2, Pt/SIPO/Pt).", "It is postulated that the electrolytes deposited with the same deposition process have identical microstructures [20].", "As shown in Figure 3a,b, both the 850-nm-thick dense GDC and SIPO electrolytes did not show any evident pinhole.", "However, the OCV of approximately 0.3 V for cell 1 was significantly lower than that for cell 2 (approximately 1.0 V).", "This result indicates that the lower OCV of the GDC-based cells may have originated from oxygen permeation through the GDC electrolyte and/or ceria reduction, not from gas leakage through pinholes.", "In order to verify the effect of the ALD YSZ layer, we characterized electrochemical performances of GDC/YSZ bilayered thin-film fuel cell (cell 3, Pt/GDC/YSZ/Pt), which has a 40-nm-thick ALD YSZ layer at the anodic interface as shown in Figure 4.", "As expected, the OCV of cell 3 with the ALD YSZ layer stayed at a decent value of approximately 1.07 V, unlike that of cell 1 (approximately 0.3 V).", "This discrepancy indicated that the ALD YSZ layer played a successful role as a functional layer to suppress the issues that originated from thin-film GDC electrolyte such as the electronic current leakage and the oxygen permeation [15-17].", "The thicknesses of GDC layers in cells 1 and 3 were 850 and 420 nm, respectively.", "Originally, it was intended for the comparison of the two samples with the same GDC thickness, but a 420-nm-thick GDC-based cell showed highly unstable outputs in the measured quantities.", "While the peak power density of the cell (cell 3) with an YSZ blocking layer reached approximately 35 mW/cm2, that of the single-layered GDC-based cell (cell 1) showed a much lesser power density below approximately 0.01 mW/cm2, as shown in Figure 5a,b.", "Figure 3 FE-SEM cross-sectional images of cells 1 and 2.", "(a) A GDC single-layered thin-film fuel cell (cell 1) and (b) a SIPO single-layered thin-film fuel cell (cell 2).", "Figure 4 FE-SEM cross-sectional image of a GDC/YSZ bilayered thin-film fuel cell(cell 3).", "Figure 5 Electrochemical performances of cells 1 and 3.", "(a) A 850-nm-thick GDC electrolyte fuel cell (cell 1) and (b) a 460-nm-thick GDC/YSZ electrolyte fuel cell (cell 3) measured at 450°C.", "To evaluate the stability of GDC/YSZ bilayered thin-film fuel cell (cell 3), the OCV and the peak power density were measured for 4 h at 450°C, as shown in Figure 6.", "While reduction of the OCV was negligible, the peak power density sharply decreased by approximately 30% after 4 h.", "This sharp performance degradation in the AAO-supported thin-film fuel cells was previously studied by Kwon et al. [32].", "They ascribed the reason to the agglomeration of the Pt thin-film without microstructural supports.", "In line with the explanation, the agglomeration of Pt particles was clearly visible when comparing the surface morphologies before and after a cell test, and the degradation of power output caused by the Pt cathode agglomeration was also confirmed through AC impedance measurements.", "Nevertheless, the stability of AAO-supported GDC/YSZ thin-film fuel cells was relatively superior to ‘freestanding’ thin-film fuel cells with silicon-based substrates [33].", "Actually, the configuration of the AAO-supported thin-film fuel cells was maintained after 10 h at 450°C.", "However, it was reported that freestanding thin-film fuel cells were all broken before 1 h in the same operational conditions [29,33].", "Figure 6 OCV and peak power density of GDC/YSZ thin-film fuel cell(cell 3)versus dwell time at 450°C.", "Conclusions In this study, we implemented and suggested a promising feasibility of a thin-film low-temperature SOFC using a bilayered electrolyte configuration on the AAO platform.", "GDC has suffered from its chemical instability and the resulting electronic leakage under a reduction environment.", "In a thin-film configuration for securing a decent oxygen ion conductivity even at low temperatures (as an LT-SOFC), oxygen permeation through the GDC film became problematic as well.", "This paper reports that an insertion of a very thin ALD YSZ layer between the anode Pt and the GDC electrolyte significantly improved the electrochemical performance of a cell.", "At 450°C, a thin-film fuel cell with 850-nm-thick GDC electrolyte showed an OCV of approximately 0.3 V and a power density of approximately 0.01 mW/cm2.", "On the other hand, a thin-film fuel cell with a bilayered electrolyte consisting of a 40-nm-thick YSZ and a 420-nm-thick GDC reached an OCV of approximately 1.07 V and a power density of approximately 35 mW/cm2.", "From these results, it was confirmed that the YSZ layer successfully acted as a protective layer.", "The cell performance is expected to further improve through the microstructural optimization of electrode interfaces and adjustment of chemical compositions of each film.", "While the fully functional YSZ layer presented here is already very thin (40 nm), there are good chances of reducing the thickness even further considering that a theoretical approach predicted an YSZ-to-GDC thickness ratio of 0.01% would suffice to guarantee electron blockage [30].", "Competing interests The authors declare that they have no competing interests.", "Authors’ contributions SJ designed the experiment, carried out the experimental analysis, and drafted the manuscript.", "IC and YHL participated in experimental measurements.", "JP and JYP carried out the growth and optimization of thin-film materials.", "MHL provided useful suggestions and improve the manuscript.", "SWC supervised the research work and finalized the manuscript.", "All authors read and approved the final manuscript.", "Authors’ information SJ and IC are students in the Graduate School of Convergence Science and Technology, Seoul National University.", "YHL, JP, and JYP are graduate students in the School of Mechanical and Aerospace Engineering, Seoul National University.", "MHL is a professor in the School of Engineering at the University of California, Merced.", "SWC is a professor in the School of Mechanical and Aerospace Engineering, Seoul National University." ]

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[ "Recent Developments of Electrochemical Promotion of Catalysis in the Techniques of DeNOx Recent Developments of Electrochemical Promotion of Catalysis in the Techniques of DeNOx TangXiaolong 1 2 http://orcid.org/0000-0001-9769-7323XuXianmang 1 YiHonghong 1 2 *ChenChen 1 WangChuan 1 1College of Environmental Science and Engineering, Kunming University of Science & Technology, Kunming 650093, China 2Civil and Environmental Engineering School, University of Science and Technology Beijing, Beijing 100083, China *Honghong Yi: yihonghong@tsinghua.org.cn Academic Editors: S.", "Niranjan and L.", "Wang 463160 Electrochemical promotion of catalysis reactions (EPOC) is one of the most significant discoveries in the field of catalytic and environmental protection.", "The work presented in this paper focuses on the aspects of reaction mechanism, influencing factors, and recent positive results.", "It has been shown with more than 80 different catalytic systems that the catalytic activity and selectivity of conductive catalysts deposited on solid electrolytes can be altered in the last 30 years.", "The active ingredient of catalyst can be activated by applying constant voltage or constant current to the catalysts/electrolyte interface.", "The effect of EPOC can improve greatly the conversion rate of NOx.", "And it can also improve the lifetime of catalyst by inhibiting its poisoning. http://dx.doi.org/10.13039/501100001809 National Natural Science Foundation of China NSFC-21177051 1.", "Introduction In the 1970s, it has been shown that solid electrolyte played an important role in the heterogeneous catalytic.", "And the authors provided a measurement method of the oxidation degree of catalyst surface with the solid electrolyte doped ZrO2 [1].", "In the late 1970s, Vayenas and Saltsburg [2] provided a concept of solid electrolyte potentiometry (SEP) which was used widely in the research of catalysis reaction mechanism on metal surface.", "These studies were helpful for the providing of EPOC.", "The phenomenon of EPOC was firstly reported by the group of Stoukides and Vayenas [3] at MIT in 1981.", "As a result, the actual enhancement of the catalytic activity was much higher than that estimated by the Faraday law.", "They called this phenomenon nonfaradaic electrochemical modification of catalytic activity (NEMCA).", "In the later research, scholars called it for EPOC.", "In the last 30 years, it has been reported with more than 80 different catalytic systems that the catalytic selectivity and activity of catalytic active ingredient deposited on solid electrolyte can be altered greatly by applying constant voltage or constant current to the catalyst/electrolyte interface.", "The induced steady state conversion rate can be up to 150 times higher than the normal catalytic rate (open circuit) [4].", "And it can be up to 3 × 105 higher than the steady state rate of ion supply [5].", "Because of the tightening legislation related to exhaust emissions, the removal of flue gas from exhaust duct has become increasingly important.", "As one of the main pollutants, NOx originating from automotive traffic and industries, especially in urban areas, has been a research emphasis.", "The traditional technology of three-way catalytic is ineffective for the removal of NOx under lean-burn conditions.", "And the normal techniques of DeNOx face three challenges.", "The most important one is to reduce or even remove the use of noble metals (Au, Pt, Pd, Rh, Ag, etc.) because of their excessive cost which makes necessary stages of recycling and recovery.", "Another point is to improve the lifetime of the catalysts by inhibiting their poisoning under operating conditions.", "The last crucial point is how to reduce the operating temperature.", "Thus, a new type of catalytic system for effectively cleaning the flue gas under lean-burn conditions is urgently needed.", "As one of the novel technology in the field of catalytic, the EPOC has some advantages compared with the traditional catalytic.", "Different obvious advantages of EPOC will be described such as the promotion of the catalytic activity and selectivity at low temperature, the improvement of the catalytic lifetime, and the enhancement of controllability.", "Most of the literature of EPOC were was reported for the study of catalytic application and the modification of catalysts.", "However, there is not a recapitulative article only for electrochemical promoted DeNOx.", "The objective of this paper is to make the overview for the special performance of EPOC at different influencing factors and its potentialities in the field of De-NOx by describing different examples. 2.", "Reaction Mechanism The term EPOC was used to describe the phenomenon that the pronounced strongly nonfaradaic and the reversible changes in the catalytic activity and selectivity of conductive catalysts deposited on solid electrolytes.", "Vayenas et al. [6] have provided a theoretical basis and a detailed account of the phenomenology, which made the EPOC clear.", "The operating process usually requires electrochemical pumping of ions to the interface of porous working electrode and solid electrolyte.", "As a result, the modification in work function changed the activation energy of reactions and the adsorption enthalpy of adsorbed species.", "Controlling voltage provides control of the concentration of spilt over promoter species on the solid electrolyte surface.", "Therefore, the metal electrode, as catalytically active locus, is usually in the form of an electronically conducting and porous metal plate placed on the solid electrolyte.", "Catalyst structure schematic drawing is outlined in Figure 1.", "The idea of reducing NOx with electrochemical method in a solid-state cell was firstly suggested by Pancharatnam et al. in 1975 [7].", "The authors suggested that the reduction of NO occurred on the zirconia surface, even interface between electrode and solid electrolyte, and not on the electrode itself.", "The NOx received e− and was vented in the form of gaseous nitrogen to air.", "The Ov− was transferred through the solid electrolyte to metal anode plate and vented in the form of O2.", "Researches made it clear that this process was more facile reaction under oxidizing conditions [8].", "The cathode had a high activity and selectivity towards the reduction of NOx when O2 was present along with NOx.", "The result showed that the reduction rate of NOx exceeded that estimated with the Faraday law by a thousand fold under a high cathodic overpotential condition.", "Taking that into account, the mechanism below was proposed by the authors: (1) V o • • ( s ) ⟷ V o x ( s ) + 2 h electrode • NO + V o • • ( s ) → N − O o x ( s ) NO + N − O o x ( s ) → N 2 O + O o x ( s ) N 2 O + V o x ( s ) → N 2 + O o x ( s ) O o x ( s ) + V o • • ⟷ V o • • ( s ) + O o x ( b ) , where Vox is a F-center, (s) the surface of electrolyte, and (b) the bulk of the electrolyte.", "This hypothesis was authenticated by Gür and Huggins using Pt and Au point electrodes in the later work [9].", "In a work by Gessner et al. [10] in 1988, the authors suggested that oxygen conversion was not always the dominant charge transfer reaction.", "The oxidation of nitric oxide to nitrogen dioxide and the reduction of nitrogen dioxide to nitric oxide were found to be the dominant charge transfer reactions in their work.", "Three parameters usually describe the magnitude of electrochemical promotion: (1) the rate enhancement ratio (ρ) defined from (2) ρ = r r o , where r is the electropromoted catalytic rate, ro the unpromoted catalytic rates, (2) the faradaic efficiency (Λ) defined from (3) Λ = Δ r ( I / 2 F ) , where Δr is the potential or current induced change in catalytic rate, I the applied current, F the Faraday's constant, (3) the promotion index (PIj) of the back-spillover promoting species defined from (4) P I j = Δ r / r o θ j , where θj is the coverage rate of the promoting species (j) on the catalyst surface.", "A reaction that exhibits electrocatalysis is limited to |Λ| ≤ 1, while electrochemical promotion when |Λ| > 1.", "A reaction is termed electrophilic when Λ < −1, while electrophobic when Λ > 1.", "In the former case, the rate decreases with catalytic potential, U, while in the latter case the rate increases with catalytic potential.", "Λ values up to 3 × 105 [11] and ρ values up to 1 × 103 [12] have been found for several systems.", "Solid oxide fuel cells (SOFCs) show good results for lean NOx emission control of high-concentration NOx with or without power generation in Ta-Jen Huang's research [13–18].", "The simplified catalytic system, without consuming any reductant, that a new generation catalytic converter (electrochemical-catalytic cells, ECCs) can have a very compact size to be used for lean-burn motor vehicles [19–21].", "Authors offered the transformation process of ions on the catalysis (shown in Figure 2) [22].", "They think that either the SOFC or the ECC is by direct NO decomposition because there is no reductant over the cathode.", "The mechanism was suggested as below [22]: (5) N O 2 → NO + O NO → N + O 2 N → N 2 2 O → O 2 .", "Considering [] as the surface oxygen vacancy [23] (6) NO + [ ] · [ ] → N − [ O ] · [ ] NO + N − [ O ] · [ ] → N − [ O ] · [ O ] − N N − [ O ] · [ O ] − N → N 2 + [ O ] · [ O ] [ O ] · [ O ] → O 2 + [ ] · [ ] , where []·[] is a pair of adjacent surface oxygen vacancies and [O] denotes O in the surface oxygen vacancy, When CO2 and H2O are present in this catalytic system [22]: (7) C O 2 + [ ] → CO + [ O ] NO + ∗ − [ ] → N ∗ − [ O ] CO + N ∗ − [ O ] → C O 2 + N ∗ − [ ] H 2 O + [ ] → H 2 + [ O ] H 2 + N ∗ − [ O ] → H 2 O + N ∗ − [ ] , where ∗ denotes the active site for NO adsorption via N.", "The products are only one N species which should be distantly distributed.", "The surface diffusion of N species would influence the production of N2 in the low NOx concentration region.", "When a reductant (e.g., C3H6) is used in this catalytic system [24], (8) N O ( g ) → N O ( ads ) C 3 H 6 ( g ) → C 3 H 6 ( ads ) O 2 ( g ) → 2 O ( ads ) N O ( ads ) → N ( ads ) + O ( ads ) N ( ads ) + N ( ads ) → N 2 ( g ) N ( ads ) + N O ( ads ) → N 2 O ( g ) C 3 H 6 ( ads ) + 9 O ( ads ) → 3 C O 2 ( g ) + 3 H 2 O ( g ) .", "Comparing all the previous mechanism analysis, we may safely draw the conclusion that the electrochemical catalytic process can be divided into the following several steps: (I) the adsorption of reactant gas; (II) gas molecules combined with the active site; (III) the forced transfers of specific ions due to the effect of supplied voltage; (IV) the mutual restructuring of adsorbed ions, then desorption.", "The electrochemical catalytic efficiency is influenced by the steps (II) and (III), while the selectivity of products is related to the last step. 3.", "Influencing Factors 3.1.", "Types of Electrode and Solid Electrolyte At the present, noble metals are used as electrode plate mainly including Au, Pt, Pd, Rh, Ag, and Ir [7, 9, 25–32].", "There are special d electronic configurations in the outer electrons of these noble metals.", "This configuration provides coordination bond for the reactants on the catalyst/electrode interface.", "Reactants are activated by the coordination bond during the reaction process.", "Therefore, the noble metals materials have became the targets of preferred study.", "However, some scholars have begun to search for cheap materials to replace these noble metals because of their excessive cost which makes necessary stages of recycling and recovery.", "The cheap metal oxides CuO and NiO were studied in some papers [33, 34].", "The result showed that NiO has few activities towards the reduction of NO.", "Nevertheless, CuO is highly active towards the electrochemical reduction of NO.", "It is the same phenomenon as that observed for the traditional catalytic reduction of NO on these two oxides.", "And it is known that CuO has a better catalytic activity than NiO [35, 36].", "These papers made it clear that the bond breaking of NO was one of the restrictions for the electrochemical reduction of NO.", "The result also showed that the reduction rate of NO was increased when NiO reduced to Ni metal, whereas the reduction rate of oxygen was restrained when Cu was presented as CuO.", "Yet the reduction of oxygen was induced when CuO was reduced to Cu2O.", "Furthermore, other scholars have done a lot of work towards solid electrolyte.", "It was shown that the solid electrolyte is indispensable in the process of heterogeneous electrochemical catalysis reduction of NOx.", "The working principle of solid electrolyte in the process of EPOC has been expounded in reaction mechanism (Section 2).", "It will be expounded with an example in the next moment.", "For the solid electrolyte of O2− conductor supports, the action of EPOC has been found to derive from the anionic transfer (reverse spillover) of Oδ− species (Figure 3) [37].", "These Oδ− species together with their image charge in the metal formed a whole neutral double layer at the metal-gas interface.", "Both chemisorptions and catalysis are affected by the back-spillover and the image charge in a pronounced manner.", "The back spillover Oδ− species are different from oxygen adsorbed from the gas phase under a high oxygen condition [38–40].", "They are also less against catalytic oxidations than gas supplied oxygen.", "The EPOC effect has been confirmed for a wide field of reactions in the reduction of NOx when the electrodes are connected to a solid electrolyte.", "Electrochemical promotion was also observed on oxides such as CuO [33], RuO2 [41], and IrO2 [42].", "Several parts of literature [43–47] have reported that the using the class of oxides, the based electrodes were spinels, as cathodes for the electrochemical reduction of NOx.", "A research result reported by Wachsman et al. [48] manifested that an La0.8Sr0.2Co0.9Ru0.1O3−δ cathode had a higher conversion rate in reducing NOx than a Pt-based cathode under oxidizing conditions.", "This phenomenon was attributed to the good electrochemical catalytic characters of the perovskite-based cathode compared to the Pt-based cathode.", "In this kind of study, the solid electrolyte may be mixed ionic-electronic conductors (CeO2 [49] and TiO2 [50]), F− conductors (CaF2) [51], O2− conductors (YSZ (Y2O3-stabilized ZrO2)) [52–54], H+ conductors (Nafion [55] or CaZr0.9In0.1O3−α [56, 57]), and Na+ conductors (β′′-Al2O3 [58, 59] or Na3Zr2Si2PO12 [60]).", "It is also a good research field that coating of metal based electrodes. 3.2.", "Configurations of Electrochemical Promotion Reactors Electrochemical promotion has been studied for over eighty different catalytic systems [37], while it has mainly two kinds of forms of electrochemical promotion reactors classified in structures.", "One is to which the reactor only working electrode is exposed in the reactant gas (Figure 4).", "The other is the reactor that both electrodes and solid electrolyte were exposed in reactant gas (Figure 5).", "The porous catalyst film or working electrode of the reactor shown in Figure 4 is exposed in gas mixture, while counter electrode is exposed in air.", "Because the process of EPOC just occurred on the surface area of the film, the reactor shown in Figure 4 has more advantages compared with the reactor shown in Figure 5 in the mechanism research of EPOC.", "In the paper by Song et al. [61], the cathode was assembled in a bilayer structure.", "The Pt paste was screen-printed as a circle on the yttria stabilized zirconia (YSZ) disk.", "The anode was also the platinum applied on the other side of the solid electrolyte.", "Then, metal lines were contacted with the platinum layers at both sides.", "In the consideration of impedance measurements, the platinum reference electrode applied on the opposite side of the working electrode was used.", "The result showed that the reduction behavior of NO presents a function of the applied current for the electrochemical promotion cells.", "It required a threshold current to arouse the EPOC behavior of NO for all the cells.", "The EPOC behavior of NO did not occur if external current was applied insufficiently.", "Its conversion rate was increased abruptly when a higher current density was supplied to the cell.", "It is feasible that the conversion rate of NO reach to 87% at 250 mA/cm2, although this reaction started at 60 mA/cm2.", "In contrast, all the counter electrode, working electrode, and solid electrolyte of the reactor shown in Figure 5 are exposed in the gas mixture.", "The catalytic active sites spread over carrier contact easily with gas mixture compared with another one.", "Based on the previous advantage, the reactor shown in Figure 5 has a higher value in the EPOC applied research.", "In the paper by Dorado et al. [24], the EPOC reactor was made of a pyrex tube.", "And the catalytic experiments were operated at atmospheric pressure.", "The catalytic reaction process was carried out in this kind of tubular solid electrolyte reactor.", "The temperature of catalytic reaction was detected with a K-type thermocouple installed inside the inner of reactor.", "And the external heat producer of the EPOC reaction was a furnace outfitted with a heat control system.", "The result showed that the system in catalytic potential modification on reaction rates could be electrochemically promoted.", "The conversion rate of NO was increased at low O2 concentration (0.5 and 1%) under the traditional optimally promoted conditions.", "However, it could be seen that the conversion rate of NO was decreased when the O2 concentration increased, eventually resulting in an entire loss.", "The increase of O2 concentration results in a decreasing of the efficiency of EPOC for NO reduction.", "This phenomenon could be attributed to that a relative increase of the surface coverage of O2 and a strong inhibition of the reductant adsorption.", "Although the EPOC has been studied for more than 30 years, there has been no large-scale commercial operation.", "It is chiefly because of the lack of compact and efficient reactor designs allowing for the operation of EPOC.", "In the paper by Balomenou et al. [62], a novel dismountable monolithic-type EPOC reactor and an ingenious sensor-catalytic reactor unit have been designed and tested for the reduction of NO by C2H4 under an oxygenic condition (Figure 6).", "The reactor can be considered as a complex between a ribbed-plate or flat-plate solid oxide fuel cell and a traditional monolithic honeycomb reactor.", "Two external electrical connections were required in this novel reactor.", "And the novel reactor achieves easily practical utilization of the EPOC.", "In this novel reactor, thin (about 20 ~ 40 nm) porous catalyst films were made of two different materials (Au and Rh, Pt and Rh).", "These films are sputter-deposited on the opposing surfaces of solid electrolyte.", "The shapes of solid electrolyte are thin (0.25 mm) parallel plates.", "And the solid electrolyte parallel plates were supported in the grooves of a ceramic monolithic holder.", "The Au/YSZ/Rh-type serve as sensor elements and the Pt/YSZ/Rh-type as electrochemical promoted catalyst elements.", "The 22-plate reactor was tested under high flow rate (1.8 L/min) and gas hourly space velocity (1200 h−1) condition.", "This novel reactor could achieve higher conversions (about 90%) than all former electrochemical promoted catalysis units and showed significant promise for the commercialization and practical applications of EPOC. 3.3.", "With or without Reductant The EPOC can be divided into two categories according to whether the reductant is consumed.", "The unsaturated hydrocarbon compounds (HC) is usually used as reductant.", "Notably, propylene is usually used to represent HC in the engine exhaust [63].", "The selective catalytic reduction of NO by C3H6 was investigated by Constantinou et al. [27].", "His group studied the effect of EPOC on porous polycrystalline Rh catalyst-electrode films.", "The result showed that the rate of NO reduction and CO2 formation was enhanced, respectively, by factors of up to 55 and 200 due to the application of current or potential between the Rh catalyst-electrode and an Au counter electrode.", "Huang et al. [64] attempt to clear simultaneously NOx and hydrocarbons with electrochemical catalytic.", "The result showed that a higher oxygen concentration is beneficial to both the NO conversion and the hydrocarbons oxidation to result in zero pollution.", "The effect of adding propylene for NO removal was also investigated (result shown in Figure 7).", "Figure 7 shows that both adding propylene and decreasing temperature increase the NO removal.", "Moreover, The effect of decreasing temperature from 450 to 400°C is smaller than that of adding 350 ppm propylene.", "The effect of adding propylene is similar to that of HC-DeNOx over catalyst [65].", "NOx can be reduced by propylene.", "Besides, C3H6 [66–68], many other species of HC (including CH4, C2H4, C3H8, and C5H12) [69, 70] were investigated.", "The results showed that the presence of HC is favorable for NOx removal.", "This electrochemical promotion is also present at the catalytic system that CO [71] or NH3 [72] is reductant.", "But the presence of reductant may inhibit other forms promotion in same times.", "In the paper reported by Dorado et al. [24], the effect of EPOC for the reduction of NO by C3H6 was studied.", "This effect was firstly investigated on a Pt impregnated catalyst film directly deposited onto an Na-β′′-Al2O3 solid electrolyte.", "The result showed that the presence of promoters enhanced the selectivity of N2.", "However, combined with characterization results, the promotional effect of sodium on the overall catalytic activity for NO removal would be inhibited when C3H6 and O2 are present.", "Authors thought that the phenomenon can be attributable to the result of a strong inhibition of C3H6 adsorption and a relative increase of the O2 coverage.", "The electrochemical promotion of decomposition is an effective method for NOx removal.", "In 2001, the electrochemical cells of oxide|Pt (cathode|YSZ|Pt (anode) for NO decomposition were designed and investigated [73].", "It was shown that the properties of the electrochemical cell for NO decomposition and the value of the current efficiency could be enhanced because of the specific microstructure of the NiO-YSZ mixed oxide.", "And an electrochemical cell for NO decomposition was firstly designed for which the value of current efficiency is exactly equal to the theoretical one.", "In the following studies, his group proved that the NO conversion was positively associated with the value of the current, while the value of current efficiency is only dependent on the NO and O2 gas concentrations [74, 75].", "It is possible to minimize the values of the cell operating voltage by the control of the composition of the (NiO)x-(YSZ)1−x electrocatalytic electrode [76].", "In 2004, his group proposed a novel electrochemical promotion reactor for NOx decomposition.", "This reactor was designed by compositional control and nanostructural of an NiO-YSZ electrochemical promotion catalytic electrode [77].", "In such reactors, the electrical power required for NO decomposition is greatly reduced in the presence of 10% of O2.", "Therefore, the energy consumption required for NO removal in such reactor is lower than that in traditional cells.", "The catalytic activity of electrochemical promotion decomposition for NOx was strongly influenced by microstructure, composition, and the configuration of the working electrode [78, 79].", "The cell composed of (La2Sn2O7 + YSZ)/Pt composite electrode was investigated by Park et al. [79].", "A higher catalytic activity of electrochemical promotion decomposition was observed for the cell composed of (La2Sn2O7 + YSZ)/Pt composite electrode than the Pt electrode.", "The result showed that 87% NOx was reduced at the current density of 194 mA/cm2 in the reactant gas containing 2% O2, while such cell decomposed 80.5% NOx at the current density of 325 mA/cm2 under 4% O2 condition.", "The cell stacks composed of Ce0.9Gd0.1O1.95 porous electrolyte and La1−xSrxMnO3 (x = 0.15, and 0.5) composite electrode were investigated by Werchmeister et al. [80].", "The cell stacks were infiltrated with the nanoparticles of Ce0.9Gd0.1O1.95, Ce0.8Pr0.2O2−δ and pure ceria after sintering.", "It is possible to reduce up to 35% of NO present when the cell stacks are polarized with 1.5 V for each cell.", "It is shown that the cell stacks infiltrated with pure ceria had the highest electrochemical catalytic activity.", "However, the highest selectivity towards NO compared to O2 present at the ones infiltrated with Ce0.9Gd0.1O1.95.", "The electrochemical promotion of catalytic deoxidation and decomposition is an effective way to NOx removal.", "The EPOC deoxidation for NOx usually has a higher NOx conversion due to the presence of reductant.", "However, the reductant should cause secondary pollution if the catalytic process is an incomplete reaction.", "The proportion of added reductant should be paid enough attention.", "The EPOC decomposition for NOx is an ingenious way to avoid the pollution caused by reductant.", "However, compared with deoxidation, the conversion of NOx of the EPOC decomposition is unsatisfactory.", "Therefore, improving the NOx conversion of the EPOC decomposition would become a direction with quite development potentiality in the future. 4.", "Recent Positive Results In 1990, Cicero and Jarr [81] reported firstly the use of oxide-based electrodes in the reduction of NO.", "The authors used a metal oxide-based cathode to remove NO, which achieved a conversion of 91% with O2 concentration of 8%.", "The temperature range of experiment was from 650°C to 1050°C.", "But they did not give the magnitude of the current efficiency in this paper.", "The influence of NO for the reduction rate of O2 on La0.8Sr0.2MnO3−δ based electrodes was reported in 1995 [82].", "Reinhardt et al. found that the reduction rate of O2 was increased when NO was added to the gas mixture in the temperature range of 500 ~ 900°C.", "But they did not undertake the gas analysis when NO was added to the gas mixture.", "Therefore, it is possible that the reduction of NO itself led to the current density increased.", "In 1996, Palermo et al. [83] did a deeper research on the system used either propene or CO as reductant.", "The result showed that an obvious increase of NO reduction rate was achieved when Na+ were pumped to the catalysts surface.", "The authors made a point that the increase of NO reduction rate was related to operated temperature, applied potential, and gas composition.", "The maximum increase of NO reduction rate was achieved at 375°C when a low potential (0.25 V) was applied on the system.", "Authors thought the Na+ could induce weakening of the NO bond, which led to a easier dissociation of NO bond.", "This step played an important role in the enhancement of NO reduction rate.", "In the later research, Yentekakis et al. [84] found that the reduction of NO with propene was observably enhanced when Na+ was pumped to the Pt surface.", "In conclusion, authors thought this enhancement in the reduction of NO owed to a sodium-induced promotion of the NO bond dissociation.", "In 1997, a paper reported by Marina et al. [85] narrated the reduction of NO with H2 using a Pt catalyst on β′′-Al2O3 Na+ conducting solid electrolyte.", "The research showed that the electrochemical promoted catalytic reduction rate of NO was increased up to 30 times more than the unpromoted catalytic rate.", "What is more, the electrochemical promoted catalytic reduction rate of NO was increased with over thousands times more than the rate of Na+ pumped to the catalysts surface.", "At the same time, the catalytic selectivity of NO to N2 was increased from 30% to 75%.", "In 1999, a research reported by Belyaev et al. [86] investigated the electrochemical promoted reduction of NO with CO.", "In this research, authors used Pt material as catalysts supported on YSZ.", "The result showed that the reduction rate of NO was strongly increased when the current was applied to cathodic.", "In the research published in 2000, Kaneko et al. [87] found that NO could be reduced at 800°C after being injected in pulses.", "Authors used a platinum electrode placed on the YSZ and provided relatively high potentials (−500 mV versus air) to the system.", "In the study by Hibino et al. [88], it was shown that the alternating current efficiency was highest when the applied potentials were higher than 3 V in combination with the use Pd electrode.", "However, the direct current efficiency was highest when the applied potentials of lower than 3 V.", "In 2001, Bredikhin et al. [73] attempted to use a multideck electrode structure.", "The multideck electrode structure consisted of an NiO/YSZ electropromoted catalytic active layer, a YSZ covering layer and a Pt/YSZ cathode.", "The result showed that the activity of the cathode layer was related to the Pt/YSZ ratio.", "In 2003, a paper reported by Vernoux et al. [89] narrated that the platinum was supported on NASICON which was a kind of Na+ conducting electrolyte.", "And the propene was used as reductant for the reduction of NO.", "The result showed that the reduction rate and the selectivity of NO to N2 was increased when a low potential (100 mV) was applied on the system.", "It is possible that nitric oxide was efficiently reduced at low temperature of 300°C.", "The use of the NASICON electrolyte made it possible that the electrochemical promoted catalysis reaction was operated at a low temperature.", "In the research by Petrushina et al. [90], a proton conducting H3PO4 based electrolyte was used to the reduction of NO at a lower temperature (135°C).", "The H2 was used as reductant in this electrochemical promoted catalysis system.", "The result showed that the reduction rate of NO could be enhanced when the Pt electrode was provided a negative potential.", "In 2005, Kammer and Skou [91] studied the Fe-Mn-based perovskites catalyst.", "From their research, the result showed that the Fe-rich perovskites had the highest catalytic activity in the reaction of the electrochemical promoted reduction of NO.", "This result identified with the hypothesis that the reduction rate of NO was determined by the amount of oxide ion vacancies and the redox capacity.", "However, in another paper by Simonsen et al. [92], the catalytic activity was decreased after adding BaO to the perovskites-based electrode.", "In this research, the catalytic selectivity was also investigated.", "In the conclusion, the authors presented that the selectivity was strongly enhanced after adding BaO to the perovskites-based electrode.", "In 2006, the influence of the YSZ covering layer was studied again by Hamamoto et al. [93].", "The result showed that the YSZ covering layer led to the suppression of the adsorption and the decomposition of O2.", "In 2008, the multideck electrode structure was studied by the same group of Hamamoto et al. [94].", "In this research, the top of the multideck electrodes applied an extra-covering layer.", "This covering layer consisted of Na, K, or Cs together with Pt and Al2O3, which were used as NOx adsorbing layer.", "At last, it was shown that the adsorbing layer containing K appeared a better effect than others.", "This type of cathode in the paper could achieve a quite high catalytic activity.", "And it is possible that the conversion of NOx is increased about 20% due to the current effect.", "Therefore, this type of multideck electrodes is a developed direction in the research of removing NOx.", "The effect of EPOC can be used to activate a metal catalyst for the selective catalytic reduction of NOx under wet reaction conditions.", "In 2009, the effect of some operating conditions on the simultaneous removal of NOx and SO2 was investigated.", "The simulated NO-SO2-air flue-gas mixtures were bubbled into a integrated wet scrubber electrochemical cell system in Il-Shik Moon's research [95].", "The result showed that the NOx was fast and greatly reduced when SO2 coexisted in the scrubber column.", "And it was proved that the SO2 removal from the NO-SO2 mixture occurred independent of NOx with no interference what so ever.", "In the paper reported by de Lucas-Consuegra [96], the catalytic performance of Pt electrode can be optimized by the application of different potentials at each operation temperature.", "The catalytic behavior of the system is optimized due to the combined use of the Pt/K-βAl2O3 cell under changing reaction conditions.", "The effect of voltage and temperature on NO removal with power generation in a solid oxide fuel cell (SOFC) unit was investigated in 2010 [97].", "The SOFC is constructed with Ni-(Ce,Gd)O2−x as anode, YSZ as electrolyte, and V2O5-added (LaSr)(CoFe)O3-Ni-(Ce,Gd)O2−x as cathode.", "It is shown that the NO conversion increases slightly with the decreasing voltage but with increasing temperature from 800°C to 875°C.", "And the NO conversion increases as O2 and NO concentrations decreases when the process is operational under 2–5% O2 concentration condition.", "In the paper reported by Hadjar et al. [98], an electrochemical NOxTRAP catalyst Pt-Ba/YSZ was investigated.", "The NOxTRAP catalyst is one of the technology of DeNOx [99].", "It is shown that the cathodic polarization is beneficial to the NOx storage even under lean-burn conditions.", "The experiment was operated at 500°C with different O2 partial pressures.", "The duration until full NOx storage was drastically enhanced about 80 times in the presence of 6% O2.", "And NOx can be reduced about 10% due to the occurrence of electrochemical reduction during regeneration phases.", "Authors thought that the generation of oxygen vacancies on the YSZ surface induced by negative polarization is the major influence factor related to the electrochemical activation of the NOx storage capacity.", "An ingenious multilayer electrochemical cell was investigated in 2012 [100].", "An ytrria stabilized zirconia cover layer was replaced with an adsorption layer of the cell.", "It is shown that the electrochemical properties of NOx removal were dramatically enhanced.", "Authors thought that the enhancing of the NOx removal was related to the following two aspects: the extensive release of selective reaction sites for NOx species, a strong promotion for NOx reduction as adsorption layer connected with both the Pt and catalytic layers.", "The optimizing of electrochemical cell may provide a promising direction for NOx emission control [101]. 5.", "Conclusions It has been shown that the catalytic activity and selectivity of a few catalytic reactions can be modified by electrochemical promotion.", "Many studies have been reported related to the effect of EPOC during the last 30 years.", "The study about its mechanism and application is becoming a trending topic in the field of reduction NOx.", "It is possible that the electrochemical promotion reduction of NOx was operated in a few types of solid-state electrochemical cells.", "It was reported that the cathode materials or catalysis species with an enough coordination bond were effective for the electrochemical promotion reduction of NOx.", "The importance of the EPOC phenomenon both in electrochemistry and catalysis was highlighted with the effectiveness of EPOC for catalytic oxidations and reductions using different types of catalysts, electrodes, and solid electrolytes.", "Further development of catalysts, electrodes, and solid electrolytes materials are needed in order to increase the reduction rate of NOx.", "The improving lifetime of the catalysts also appears quite promising.", "The development of large-scale novel monolithic applicable reactors with ingenious design may be beneficial to the practical utilizations of EPOC." ]

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[ "Single Sublattice Endotaxial Phase Separation Driven\nby Charge Frustration in a Complex Oxide Single Sublattice Endotaxial Phase Separation Driven by Charge Frustration in a Complex Oxide DemontAntoine†⊥SayersRuth†⊥TsiamtsouriMaria A.", "†⊥RomaniSimon‡ChaterPhilip A.", "†NiuHongjun†Martí-GastaldoCarlos†XuZhongling†DengZengqiang†BréardYohann§ThomasMichael F.", "∥ClaridgeJohn B.", "*†RosseinskyMatthew J.*† †Department of Chemistry, University of Liverpool, Liverpool L69 7ZD, United Kingdom ‡ Department of Engineering, University of Liverpool, Liverpool L69 3GH, United Kingdom §Laboratoire CRISMAT, 6 Boulevard Maréchal Juin, 14050 Caen Cedex 4, France ∥Department of Physics, University of Liverpool, Liverpool L69 7ZE, United Kingdom m.j.rosseinsky@liv.ac.uk; claridge@liv.ac.uk Complex transition-metal oxides are important functional materials in areas such as energy and information storage.", "The cubic ABO3 perovskite is an archetypal example of this class, formed by the occupation of small octahedral B-sites within an AO3 network defined by larger A cations.", "We show that introduction of chemically mismatched octahedral cations into a cubic perovskite oxide parent phase modifies structure and composition beyond the unit cell length scale on the B sublattice alone.", "This affords an endotaxial nanocomposite of two cubic perovskite phases with distinct properties.", "These locally B-site cation-ordered and -disordered phases share a single AO3 network and have enhanced stability against the formation of a competing hexagonal structure over the single-phase parent.", "Synergic integration of the distinct properties of these phases by the coherent interfaces of the composite produces solid oxide fuel cell cathode performance superior to that expected from the component phases in isolation. document-id-old-9 ja403611s document-id-new-14 ja-2013-03611s ccc-price Introduction Assembly of separate phases within a single bulk grain is important in the production of structural and functional materials: it can determine the mechanical properties of steels1 and optimize thermoelectric performance.2 Vertical nanocomposites in heteroepitaxial thin films3 enable combination of the properties of the component phases.4 In the field of complex transition-metal oxides, chemical control and optimization of properties has conventionally relied on the modification of single-phase structures by targeted substitutions.", "This has had significant impact in areas as diverse as high-temperature superconductivity, batteries, solid oxide fuel cells, magnetism, ferroelectricity, and multiferroics.", "The structures adopted by complex oxides allow fine-tuning of physical behavior by chemical substitution, for example, the use of charge reservoir layers in superconducting copper oxides to remotely control the electron count in the electronically active CuO2 planes.5 The ABO3 cubic perovskite Ba0.5Sr0.5(Co0.8Fe0.2)O3 has small dn Co and Fe cations disordered on the B-sites of an AO3 network defined by the larger Ba and Sr cations.", "It is a single-phase material because the similar charges and bonding chemistries of Co and Fe can be accommodated on a single site in the average structure, producing a combination of electronic (B-site d electrons) and oxide ion (anion vacancies) transport that makes it an effective solid oxide fuel cell (SOFC) cathode.6 In this work, we explore the effect of incorporating the highly charged d0 Mo6+ cation onto the B-site of this system.", "The distinct chemistry of this cation frustrates the formation of a single perovskite phase, as it does not match those of Co or Fe sufficiently to form single ordered or disordered distributions.", "We demonstrate the consequences of this charge frustration for the structure and properties.", "The system retains the perovskite structure by a structural and compositional phase separation, which occurs solely on the octahedral B-sites within a single AO3 matrix.", "This AO3 matrix is coherent throughout the micrometer-sized grains and templates the formation of two distinct perovskite phases.", "The dominant phase has no anion vacancies, but the endotaxial interfaces with the minority mixed ionic-electronic conductor (MIEC) phase give the nanocomposite unexpectedly good solid oxide fuel cell cathode performance.", "Experimental Section Ba0.5Sr0.5Co0.8–xFe0.2–yMox+yO3−δ samples were initially prepared by solid-state synthesis.", "Stoichiometric amounts of the starting materials were mixed together by planetary ball milling (Fritsch Pulverisette 7) for 24 hours in 2-propanol with ZrO2 balls, followed by drying, grinding, pressing into pellets, calcining at 700 °C for 6 hours, and finally heating to 900 °C for 8 hours.", "The resulting pellets were hand-ground in an agate mortar and the powder was ball-milled further for 18 hours in 2-propanol.", "After being milled, the powder was dried, ground, pressed into pellets, and subsequently sintered in air at 1000 °C for 10 hours; the grinding/pellet pressing/heating step was repeated a total of four times to achieve phase purity and good homogeneity throughout.", "Powder X-ray diffraction data were collected on a Panalytical X-pert Pro Bragg–Brentano geometry laboratory X-ray diffractometer.", "Synchrotron X-ray diffraction data were obtained on Beamline I11 at Diamond Light Source, U.K., and time-of-flight neutron diffraction (ND) data were collected on the high-resolution powder diffractometer (HRPD) instrument at the ISIS facility, Rutherford Appleton Laboratories.", "Structural parameters were refined by the Rietveld method, which is described in full in Supporting Information sections S3 and S4.", "The transmission electron microscopy (TEM) study was carried out on a JEOL JEM3010 (JEOL, LaB6 filament, 300 keV), and energy-dispersive spectrometry (EDS) data were collected on a JEM2000FX (JEOL, W filament, 200 keV).", "High-angle annular dark field (HAADF) images were collected on a JEOL JEM 2100FCs, with a Schottky field emission gun operating in scanning tunneling electron microscopy (STEM) mode with a CEOS aberration-corrected probe.", "AC impedance measurements were recorded over the frequency range 1 MHz–0.01 Hz by use of a Solartron 1260 frequency response analyzer (FRA) with a modulation potential of 10 mV, over the temperature range 873–1073 K in static air.", "The symmetrical cell was held for 90 min at each temperature to allow thermal equilibration, and measurements were made with ZPlot v.2.9b (Scribner Associates) every 50 °C.", "The impedance arcs were modeled by use of equivalent circuit models (ECM) with ZView v.3.2b (Scribner Associates).", "All experimental procedures and analysis are described in detail in the Supporting Information.", "Results and Discussion Phase Diagram Investigation The perovskite structure of Ba0.5Sr0.5(Co0.8Fe0.2)O3−δ is shown in Figure 1a.", "Incorporation of Mo6+ on the B-site affords three distinct regions—correlated with low, intermediate, and high Mo contents—within the Ba0.5Sr0.5(Co0.8–xFe0.2–yMox+y)O3−δ phase field (Figure 2a) defined by X-ray diffraction (XRD) (details of the XRD analysis can be found in Supporting Information, section S3).", "We have chosen to highlight three compositions that are characteristic of low (1), intermediate (2), and high (3) Mo content.", "Figure 1 Crystal structures of (a) single perovskite (SP) and (b) double perovskite (DP).", "A-site cations are shown as orange spheres, and B-site cations are octahedrally coordinated by oxygen (red spheres) in the ABO3 perovskite structure.", "The SP has a single B-site (shown in light blue) whereas the DP has an ordered arrangement of two different B-sites (shown in dark blue and yellow).", "Figure 2 Overview of phase assemblage and microstructure.", "(a) B-site compositions studied in the Ba0.5Sr0.5(Co0.8–xFe0.2–yMox+y)O3−δ phase field classified according to the phase assemblage observed by XRD.", "The SP region is shown in gray, SP/DP in blue, and SP/DP/BaMoO4 in red.", "The m = 4 black dashed line corresponds to a Co/Fe ratio of 4.", "Solid symbols indicate compositions for which the ASR was measured.", "The black square on the Co/Fe axis at m = 4 is the optimal composition for undoped (Ba,Sr)(Co,Fe) material (BSCF).", "Large symbols are compositions 1, 2, and 3 for which Rietveld refinements of XRD data and TEM images are shown in panels b, c, and d, respectively.", "The two points marked with crosses correspond to the SP and DP component phases refined for 2.", "(i) Rietveld refinements of XRD data and (ii) DF TEM images of representative compositions in the three regions of the phase field are shown for (b) z = 0.125 (1, SP), (c) z = 0.375 (2, SP/DP), and (d) z = 0.45 (3, SP/DP + BaMoO4) at m = 4.", "Reflection markers refer to SP (gray), DP (blue), and BaMoO4 (red); the inset shows the region where the double perovskite superstructure reflection is observed, (a wider Q-space range for the inset is given in Supporting Information Figure S3, showing the major BaMoO4 reflections).", "TEM was performed on [11̅0] oriented grains, with solely the [111]* superstructure reflections denoting the DP selected by the objective aperture.", "In the DF TEM images the darker regions are SP and the lighter regions are DP; in panel b (ii) for 1, DP domains as shown here were observed in three out of 12 crystals, with average domain size 5–10 nm over a region that is approximately 100 × 200 nm2; no DP reflections were detected by XRD.", "Supporting Information Figures S7 and S9 show that the microstructure of 2 persists throughout the SP/DP region of the phase diagram.", "Low Mo contents [x + y = z ≤ 0.15 for Co/Fe ratio (0.8 – x)/(0.2 – y) = m ≥ 4; z < 0.1 for m ≤ 2] afford a region with a single perovskite (SP) phase isostructural with Ba0.5Sr0.5(Co0.8Fe0.2)O3−δ (cell parameter ap ≈ 3.8 Å), with disordered substitution of Mo6+ onto the octahedral B-site together with Co2/3+ and Fe3/4+ [δ ≈ 0.5 in Ba0.5Sr0.5(Co0.8Fe0.2)O3−δ].7 At the m = 4 Co/Fe ratio of the Ba0.5Sr0.5(Co0.8Fe0.2)O3−δ parent, the z = 0.125 material 1 adopts this SP structure (Figure 1a).", "At intermediate Mo content (into the region marked SP/DP on Figure 2a), a second perovskite phase coexists with the SP, with a doubled perovskite (DP) unit cell (Figure 1b, cell parameter 2ap ≈ 7.6 Å) containing two distinct octahedral B-sites.", "This symmetry change is produced by cation ordering due to the size and charge differences between the first transition series dn [0.645 Å high-spin (HS) Fe3+, 0.745 Å HS Co2+]8 and the second series d0 Mo6+ (0.59 Å)8 cations.", "This phase assemblage is adopted at m = 4 by the z = 0.375 composition 2 (Figure 2c).", "Further increase in Mo content results in the third region with the expulsion of BaMoO4 (marked as SP/DP + BaMoO4) coexisting with the SP/DP mixture, represented at m = 4 by the z = 0.45 composition 3 (Figure 2d).", "Spatial Distribution and Orientational Relationship of SP and DP Phases Dark-field (DF) imaging in the transmission electron microscope (TEM) shows DP coexists with SP on the nanometer scale within individual grains in the SP/DP region of the phase diagram [Figure 2c(ii)].", "The microstructure is increasingly dominated by DP domains in the SP/DP + BaMoO4 region [Figure 2d(ii)].", "Selected area electron diffraction and DF images in the SP region [Figure 2b(ii)] reveal coexistence of pure SP grains with grains that are majority SP but contain 5–10 nm domains of the DP phase that are too small to be observed by XRD [Figure 2b(i)].", "The locations, compositions, cation distributions, and atomic-scale structures of the DP and SP intragrain components in the SP/DP material Ba0.5Sr0.5Co0.5Fe0.125Mo0.375O3−δ (2) were evaluated by TEM (grain-specific, averaging over atomic columns and showing spatial relationships) and diffraction (bulk-sensitive XRD and neutron diffraction (ND), which both provide long-range volume-weighted information).", "The individual grains (Figure 3a) consist of an intergrowth of DP and SP phases with a range of domain sizes, some reaching the order of a hundred nanometers, while other areas have a complex arrangement of smaller domains of a few tens of nanometers in size (Figure 3b).", "Fourier transforms (FT) of separate areas of a high-resolution transmission electron microscopy (HRTEM) image of a single grain of 2 (Figure 3c) show (iii) distinct SP and (iv) B-site cation ordered DP domains oriented endotaxially (the FTs of the two domains have the same relationship to the grain).", "The image shows coherent interfaces between the SP and DP components with the cation positions lying on a single lattice.", "Figure 3 Intragrain phase separation in the m = 4 SP/DP material Ba0.5Sr0.5Co0.5Fe0.125Mo0.375O3−δ (2).", "(a) Dark-field image based on the double perovskite superstructure reflections, showing DP (light) and SP (dark) domains of a range of sizes within a single grain.", "(b) Higher magnification dark-field image showing an area where the SP and DP structures coexist on the nanometer scale.", "(c) (i) HRTEM image of a [11̅0] oriented area and (ii) its Fourier-transformed (FT) diffraction pattern.", "The FT pattern is indexed as a double perovskite with the DP superstructure reflections indicated by white arrows.", "Simulation of the SP and DP regions from an HRTEM image of a single grain are shown in Supporting Information Figure S14.", "(iii) FT of a section (indicated by a white circle) of the area imaged in panel i.", "The FT diffraction pattern is indexed as a single perovskite (SP), with the absence of superstructure spots indicated by white arrows.", "(iv) FT of a second section of the same image (i), with the intense DP superstructure reflections emphasized by white arrows.", "The pattern is indexed as a double perovskite.", "The combination of images i, iii, and iv confirms the coexistence of single and double perovskite regions in individual crystallites of 2.", "Cation Distribution and Phase-Specific Crystal Chemistry ND and XRD data (Figure 4) from 2 were refined simultaneously against a model of two discrete SP and DP phases (for full details see Supporting Information Section S4): this is an approximation, as it averages over the interphase boundary volume between the two components.", "The nominal cation composition of 2 was confirmed by EDS (Supporting Information Figure S2) and used to restrain the refinement, which produced a refined global B-site composition of Co0.499(4)Fe0.125(3)Mo0.376(2).", "As required by the endotaxial domain growth, the SP and DP have closely related ap and 2ap unit cell parameters with derived ap = 3.9861(2) and 3.9899(1) Å respectively, giving 0.095% mismatch strain.", "Mo6+ is accommodated in the composite by formation of the DP (70.4(1)%; Table 1 and Figure 5a), which is based on the Co2+/Mo6+ charge-driven B-site alternation of BaCo0.5Mo0.5O3.9 The refined DP composition of Ba0.5Sr0.5(Co0.483(3)Fe0.018(2))(Mo0.453(1)Fe0.047(1))O3.00(1) is thus enriched in Mo over the global composition, with 96% and 90% occupancy of the two B-sites by Co and Mo, respectively.", "Figure 4 Final observed (black), calculated (green), and difference (brown) profiles from combined Rietveld refinement of powder diffraction data from (a) time-of-flight neutron diffraction (backscattering bank) and (b) laboratory X-rays on Ba0.5Sr0.5Co0.5Fe0.125Mo0.375O3−δ (2) nominal composition.", "Tick marks show the Bragg reflections for SP in gray and DP in blue.", "Reliability factors for the two perovskite phase model are (a) Rwp 3.88%, Rexp = 2.80%, χ2 = 1.92, RBragg(DP) = 1.97%, and RBragg(SP) = 1.52%; (b) Rwp = 6.96%, Rexp = 5.60%, χ2 = 1.54, RBragg(DP) = 3.10%, and RBragg(SP) = 3.26%.", "Fits to all banks are shown in Supporting Information Figure S6.", "Refined oxygen content was verified by iodometric titration (Supporting Information section S6).", "Table 1 Atomic Coordinates and Bond Lengths from Rietveld Refinement of Composition 2, Ba0.5Sr0.5Co0.5Fe0.125Mo0.375O3−δ (m = 4, z = 0.375) Double Perovskite Phase BaSrCo0.965(6)Fe0.129(6)Mo0.906(3)O6.00(3), a = 7.9798(3) Å weight fraction 0.7038(10), Fm3̅m (#225) atom multiplicity x, y, z Biso (Å2) occupancy Ba 8c 0.25, 0.25, 0.25 0.62(3) 0.5 Sr 8c 0.25, 0.25, 0.25 0.5 Mo 4b 0.5, 0.5, 0.5 0.15(3) 0.906(2) Fe1 4b 0.5, 0.5, 0.5 0.094(2) Co 4a 0, 0, 0 0.22(9) 0.965(5) Fe2 4a 0, 0, 0 0.036(5) O 24e 0.2594(8), 0, 0 0.63(3) 1.000(4) bond n × distance (Å) bond valence sums (Ba/Sr)–O 12 × 2.82211(3) Ba/Sr 2.81/1.79 (Mo/Fe1)–O 6 × 1.9272(7) Mo/Fe1 5.68/3.81 (Co/Fe2)–O 6 × 2.0628(7) Co/Fe2 2.20/2.64 Single Perovskite Phase Ba0.5Sr0.5Co0.539(9)Fe0.266(8)Mo0.195(2)O2.81(3), a = 3.9861(2) Å weight fraction 0.2851(8), Pm3̅m (#221) atom multiplicity x, y, z Biso (Å2) occupancy Ba 1a 0, 0, 0 0.41(6) 0.5 Sr 1a 0, 0, 0 0.5 Mo 1b 0.5, 0.5, 0.5 0.47(8) 0.195(2) Fe 1b 0.5, 0.5, 0.5 0.266(8) Co 1b 0.5, 0.5, 0.5 0.539(8) O 3c 0.5, 0.5, 0 0.89(7) 0.938(10) bond n × distance (Å) bond valence sums (Ba/Sr)–O 11.256 × 2.81863(3) Ba/Sr 2.66/1.70 (Co/Fe/Mo)–O 5.628 × 1.99307(3) Co/Fe/Mo 2.49/2.99/4.46 Figure 5 Chemical composition and cation ordering in component phases of the m = 4 SP/DP material Ba0.5Sr0.5Co0.5Fe0.125Mo0.375O3−δ (2).", "(a) Structure of the DP phase Ba0.5Sr0.5(Co0.483(3)Fe0.018(2))0.5(Mo0.453(1)Fe0.047(1))0.5O3.00(1) established from the combined refinements, viewed along the [11̅0] direction, showing cation ordering on the octahedral B-sites, which produces separate columns of distinct composition [Mo-rich site (yellow) and Mo-poor site (dark blue)] in this orientation.", "The orientation shown is the same as that in the HAADF image [panel b (ii)].", "(b) Intensity analysis of HAADF image (ii) for a [11̅0] oriented DP region of a single grain.", "(i) QSTEM multislice simulation of a vertical line scan [indicated by the red arrow in (ii) and traversing A and B-sites, corresponding to the vertical direction in panel a] according to the refined composition of the DP phase.", "A- and B-sites are labeled showing the cation ordering; BMo and BCo refer to the Mo-rich and Co-rich B-sites, respectively.", "The blue rectangles in (ii) indicate three lines of cations along which the variation of the intensity (corresponding to the horizontal direction in panel a) is shown in each case as indicated by the blue arrows to part (iii).", "Top and bottom rows correspond to B-sites (where the alternation between Co- and Mo-rich sites is clear), whereas the middle row corresponds to A-sites (homogeneous cation distribution).", "(c) SP phase Ba0.5Sr0.5Co0.539(8)Fe0.266(8)Mo0.195(2)O2.81(3) established from the combined refinements, viewed along the same [11̅0] direction.", "There is a single octahedral site.", "The orientation shown is the same as that in the HAADF image in panel d (ii).", "(d) Intensity analysis of HAADF image (ii) for a [11̅0] oriented SP region of the same grain analyzed in panel b.", "(i) QSTEM multislice simulation of a vertical line scan [indicated by the red arrow in (ii), traversing A- and B-sites and corresponding to the vertical direction in panel c] according to the refined composition of the SP phase.", "A- and B-sites are labeled, showing the absence of B cation ordering in contrast to panel b (i).", "The absence of B-site order is shown in (iii) in the top and bottom line scans (corresponding to the horizontal direction in panel c) together with the homogeneous cation distribution in the middle A row.", "Introduction of Fe3+ (oxidation state determined by Mössbauer spectroscopy; Supporting Information section S5 and Figure S12) into the 2+/6+ B-site array of the oxygen-stoichiometric DP respectively reduces and increases the charges of the Mo- and Co-based sublattices.", "In contrast to the Mo-rich character of this phase, Fe solubility in the DP is below that expected from the global composition, as it reduces the charge and composition imbalance between the B-sites and suppresses the cation order that defines this phase.", "Fe-induced defects in the B-site ordering pattern are assimilated in the composite by the formation of the Fe-rich, Mo-deficient, B-site disordered SP phase Ba0.5Sr0.5Co0.539(8)Fe0.266(8)Mo0.195(2)O2.81(3).", "This SP phase is isostructural with the parent material (Figure 5c) and, in contrast to the DP, contains anion vacancies.", "The refined O content and stability of Mo6+ in air allow the mean Co/Fe oxidation state in the SP to be calculated as +3, which with the Mössbauer determination of the Fe oxidation state as +3 gives an SP Co oxidation state of +3.", "The transition metal charges are Co3+ and Fe3+ in undoped Ba0.5Sr0.5(Co0.8Fe0.2)O3−δ,10 which has a much higher oxygen vacancy rate than the SP here.", "The reduced Mo content minimizes the occurrence of unfavorable Mo6+ near-neighbor pairs in the disordered SP.", "The global refined composition of 2 is Ba0.5Sr0.5Co0.499(4)Fe0.125(3)Mo0.376(2)O2.94(2).", "Oxygen content was verified by iodometric titration as O2.96(1) (Supporting Information section S6), in agreement with the refined composition and consistent with a thermogravimetric analysis study (Supporting Information section S7).", "The overall O content of 2 is thus higher than the 2.75–2.4 range found for Ba0.5Sr0.5(Co0.8Fe0.2)O3−δ.7,10−12 Ba0.5Sr0.5Co0.499(4)Fe0.125(3)Mo0.376(2)O2.94(2) consists of a nanoscale assembly of 70.4(1)% Ba0.5Sr0.5(Co0.483(3)Fe0.018(2))(Mo0.453(1)Fe0.047(1))O3.00(1) (DP) and 29.6(1)% Ba0.5Sr0.5Co0.539(8)Fe0.266(8)Mo0.195(2)O2.81(3) (SP).", "The observed SP/DP microstructure is persistent in the Ba0.5Sr0.5(Co0.8–xFe0.2–yMox+y)O3−δ materials because of the charge-based frustration of Mo-induced DP B-site order by Fe3+, driving the intragrain compositional and structural segregation reflected in the refined compositions of the two component phases.", "Fe3+ substitution occurs preferentially on the Mo6+ site rather than the Co site in the DP for charge balance reasons.", "This produces low Fe solubility in the DP as high Fe contents will favor SP formation, thus explaining the persistence of the DP/SP single sublattice phase separation in all the materials investigated, while the common AO3−δ network promotes intragrain coexistence, resulting in the associated microstructures.", "At the Mo content of 2, the different chemistries of the three B-site cations thus drive the formation of two phases that are compositionally and structurally distinct but are endotaxially related.", "The DP is expected to be a pure electronic conductor whereas the oxygen vacancies in the SP make it a mixed ionic-electronic conductor (MIEC), demonstrating that distinct functions are generated by the phase separation.", "The observed potential curves along the atomic columns in high-angle annular dark field (HAADF) images of different regions of a [11̅0] oriented single grain of 2 agree with multislice simulations13 based on the refined crystallographic models of each constituent phase within the composite (Figure 5b,d; details of the simulations are in Supporting Information section S8.1).", "The HAADF images show that the A sublattice is equivalent in DP and SP, whereas these regions differ in their B sublattice occupancy, in agreement with the diffraction work.", "The bulk diffraction methods further demonstrate the coherence of the AO3−δ sublattice over which the B-site compositional and site-ordering cation separation occurs through the refined A-O distances of 2.81863(3) Å (SP) and 2.82211(3) Å (DP).", "The DP O position is not fixed by symmetry, so the observed bond length match is not simply a consequence of the unit cell dimensions.", "There is thus a single Ba0.5Sr0.5O3−δ network with constant, almost unstrained (0.12%) A–O distances spanning the coherent SP and DP phases defining each grain.", "The octahedral B-sites within this network are occupied in a spatially modulated manner by the three transition metal cations.", "The separation into two structurally matched phases of distinct composition observed here is distinct from the order–disorder phenomena observed in materials such as relaxor ferroelectrics, which are compositionally homogeneous.14 This is demonstrated by the observation of two distinct sets of cell parameters in the Mo-substituted materials studied here, which relaxes strain and leaves the different chemical bonding environments for the three cations achieved by the formation of two phases as the reason for the phase separation.", "Thermal Stability of Phase-Separated and Single-Phase Materials The effect of this nanoscale single sublattice phase separation on the stability of 2 was then investigated (full details in Supporting Information section S9).", "The stability after aging for 120 hours at 750 °C in air of Ba0.5Sr0.5(Co0.8Fe0.2)O3−δ and the Mo-substituted Ba0.5Sr0.5(Co0.8–xFe0.2–yMox+y)O3−δ phases at the constant Co/Fe ratio m = 4 is shown in Figure 6a (extended aging of 2 is shown in Figure 6b).", "The cubic perovskite structure is retained for the SP/DP composite 2, whereas there is significant decomposition of the SP materials Ba0.5Sr0.5(Co0.8Fe0.2)O3−δ and Ba0.5Sr0.5Co0.7Fe0.175Mo0.125O3−δ (1) to a hexagonal perovskite.", "DC conductivity measurements in CO/CO2 atmospheres (Supporting Information section S11) and X-ray analysis post-measurement (Figure 6b) reveal that 2 is stable to 10–10 atm O2 and under 1600 ppm CO2 at 700 °C; a reduction in lattice parameter was observed due to the loss of lattice oxygen, as observed for BSCF under similar conditions,10 but no decomposition products were visible in the PXRD pattern.", "The SP/DP stabilization of the cubic structure extends to higher Co/Fe ratios (e.g., 4, m = 10, z = 0.45).", "The B-site compositional and ordering segregation driven by Mo substitution in the SP/DP region of the phase field affords SP domains stabilized locally by enhanced Fe content over that of the global composition (higher Fe contents are known to stabilize pure cubic Ba0.5Sr0.5(Co1–xFex)O3−δ against the formation of the hexagonal phase15) together with Co/Mo-rich DP stabilized by cation ordering and the absence of anion vacancies.", "Local compositions of the two component phases emerging from the B-site occupancy modulation within the coherent cubic AO3−δ network defining the entire grain give the observed stability against the hexagonal perovskite.", "Charge frustration thus favors the cubic structure over the competing hexagonal perovskite structure.", "Figure 6 Thermal stability of perovskite structures in SP and SP/DP regions of the Ba0.5Sr0.5(Co0.8–xFe0.2–yMox+y)O3−δ system.", "(a) PXRD (logarithmic intensity scale) after aging at 750 °C for 120 h in air for Ba0.5Sr0.5Co0.8Fe0.2O3−δ (BSCF, black, SP), Ba0.5Sr0.5Co0.7Fe0.175Mo0.125O3−δ1 (gray, SP), Ba0.5Sr0.5Co0.5Fe0.125Mo0.375O3−δ2 (blue, SP/DP), and Ba0.5Sr0.5Co0.50Fe0.05Mo0.45O3−δ4 (blue, SP/DP).", "The appearance of hexagonal perovskite decomposition products is indicated by asterisks in the SP materials BSCF and 1.", "(b) PXRD patterns (linear intensity scale) showing phase stability of 2 after long-term thermal aging: Ba0.5Sr0.5Co0.5Fe0.125Mo0.375O3−δ2 was aged in air for 5 days (blue) and 10 days (purple) and aged in pO2 = 10–10 atm in the presence of ∼1600 ppm CO2 (gray).", "No new phases were detected.", "(Inset) Superposition of the 10 days and 5 days PXRD patterns in the main figure over a narrower Q range, showing that the 110 cubic perovskite Bragg reflection common to the SP and DP phases is identical after aging in air.", "Composition 2 was studied by powder X-ray thermodiffraction from 25 to 900 °C (Figure 7); above this temperature, it reacts with the quartz capillary.", "The prevalence of the domain structure was observed throughout this temperature range with little variation in phase fraction or Mo content of the SP phase (Figure 7b).", "Lattice parameters of the SP and DP phases increase linearly within a large part of the measured temperature range (Figure 7a).", "A deviation in linearity of the thermal expansion was found at lower temperatures, which can be attributed to a slight change in oxygen composition upon heating from room temperature to 500 °C, as has been observed previously for BSCF.16 The lattice parameter difference between the phases remains nearly unaltered throughout the temperature range measured.", "This reflects the clamping of the lattice parameters due to the fixed AO3−δ matrix within which the B-site compositional exchange takes place.", "This almost parallel evolution is characterized by linear thermal expansion coefficients from 500 °C that are very similar for the two phases (14.1 × 10–6 and 14.5 × 10–6 K–1 for SP and DP phases, respectively), while being smaller than values reported previously for BSCF in a similar temperature range ((19.0–22.9) × 10–6 K–1),10,16 suggesting an improved compatibility with typical ceria-based electrolytes SDC (Sm0.2Ce0.8O1.9, 11.4 × 10–6 K–1)17 and GDC (Gd0.2Ce0.8O1.9, 12.21 × 10–6 K–1)18 when compared to BSCF.", "In parallel, the size of the SP and DP domains, as determined by analysis of sample broadening, showed little deviation within this temperature range (Figure 7c).", "Moreover, the biphasic character at the synthetic temperature was confirmed ex situ with a quenching experiment from 1000 °C, evidencing a mixture of 43(3)% SP and 57(3)% DP.", "The in situ experiment also showed a rearrangement of the domain structure from 500 to 800 °C that may be correlated with the oxygen loss detected by thermogravimetric analysis (TGA) occurring in this temperature range, provoking a different charge repartition in the AO3−δ network as the average formal oxidation states of transition metals are reduced.", "Oxygen loss favors the expansion of oxygen-deficient SP domains, with a slight increase of their molybdenum content [from 0.20(2) to 0.25(2)], while DP domains are therefore contracted.", "Variation of the oxygen content is expected to have a dramatic effect on the domain structure as it is a compositional tool to influence the B-site chemical content in terms of electronic charges.", "The charge frustration maintains the observed phase separation over a wide temperature range, in contrast to the disappearance of this separation at the spinodal temperature seen, for example, in lead-based thermoelectric materials.", "Figure 7 Microstructural and compositional features from Rietveld refinements of variable-temperature synchrotron X-ray diffraction data for 2, Ba0.5Sr0.5Co0.5Fe0.125Mo0.375O3−δ (m = 4, z = 0.375).", "(a) Lattice parameter progression, expressed in terms of the single perovskite unit cell, ap.", "Linear thermal expansion coefficients in the temperature range 500–900 °C (solid line) are given, and these are extrapolated to lower temperature to show a deviation from linearity (dashed line).", "(b) SP phase fraction and Mo content refined for the SP phase.", "(c) Volume-weighted domain sizes.", "DP odd refers solely to the supercell reflections for the DP, and as such represent the volume-weighted crystallite size of the DP in absence of any antiphase boundaries that may contribute to the DP subcell reflections.", "Error bars shown are 3 times the standard deviation from the refinements; in panel a, errors on the lattice parameters are on the fifth decimal place and therefore lie beneath the plotted symbols.", "Electrochemical Properties The Ba0.5Sr0.5(Co0.8–xFe0.2–yMox+y)O3−δ materials contain MIEC component phases and are potential SOFC electrodes.", "Symmetrical cells were prepared from selected compositions in the three regions of the phase field to evaluate their SOFC cathode performance by measurement of the area-specific resistance (ASR) (Figure 8a; Supporting Information section S10 and Table S11).", "The single-phase SP parent material Ba0.5Sr0.5(Co0.8Fe0.2)O3−δ itself is an MIEC and effective SOFC cathode that displays a range of ASR values from 0.03 to 10 Ω·cm2 at 650 °C,6,19 depending on processing conditions and electrolytes.", "The aim of this study is not to produce the lowest reported ASR for Ba0.5Sr0.5(Co0.8Fe0.2)O3−δ-related cathodes but rather to examine the effect of charge frustration on structure and properties; here we measure an ASR of 0.15 Ω·cm2 for the Ba0.5Sr0.5(Co0.8Fe0.2)O3−δ parent at 650 °C with Ce0.8Sm0.2O2−δ electrolyte.", "Mo6+ is a component of heterogeneous catalyst systems involving dioxygen activation20,21 and may enhance the oxygen reduction performance of the Ba0.5Sr0.5(Co1–xFex)O3−δ family.", "Figure 8 Physical properties and cathode performance in SP and SP/DP regions of the Ba0.5Sr0.5(Co0.8–xFe0.2–yMox+y)O3−δ system.", "(a) ASR of BSCFM compositions measured in air by AC impedance of symmetrical cells represented on a logarithmic scale between 600 and 800 °C.", "Colors are selected according to the location in the phase field shown in Figure 2a: black, BSCF; gray, SP; blue, SP/DP; red, SP/DP + BaMoO4. z = x + y is the Mo content; m is the Co/Fe ratio.", "(b) ASR at constant Co/Fe ratio (m = 4) with varying Mo content z at 650 °C, highlighting the anomalous nature of the z = 0.375 composition 2 (blue diamond).", "The same symbols are used for each composition as in panel a.", "(c) DC conductivity in air for the compositions given in panel a with the same color scheme.", "The conductivity decreases with increasing Mo content.", "The linear variation with temperature for 2 indicates that the changes in composition and microstructure on heating are minor, which is confirmed by Rietveld refinement of variable-temperature synchrotron X-ray diffraction data in Figure 7 and Supporting Information section S3.5 and by TGA data in Supporting Information section S7 and Figure S13.", "ASR values measured for Mo-substituted materials range from 0.13 to 1.0 Ω·cm2 at 650 °C.", "The lowest ASR is observed for Ba0.5Sr0.5Co0.5Fe0.125Mo0.375O3−δ (2), which is located in the SP/DP region (z = 0.375) and has the Co/Fe ratio m = 4 identified as optimal in the Ba0.5Sr0.5(Co1–xFex)O3−δ family.", "The ASR of 2 is lower than that of Ba0.5Sr0.5(Co0.8Fe0.2)O3−δ between 650 and 800 °C (Figure 8a).", "In order to separate compositional and porosity effects on electrode performance, we assessed the cathode microstructure by scanning electron microscopy (SEM) imaging and determined the surface area by gravimetric methods.", "Direct measurement of the pore volume by sorption measurements is challenging22,23 due to the low masses of electrode material used relative to the dense SDC electrolyte used in the symmetrical cell configuration.", "We achieved this by using the identical screen-printing process for the cathode but onto thin Pt substrates supported on the electrolyte; once removed from the electrolyte support, this permitted gravimetric determination of N2 sorption on the Pt-supported cathode and, once the cathode is dissolved by use of 3 M HCl, the Pt substrate itself (Figure 9a).", "The surface area of the cathode coating was calculated by point-by-point subtraction between data for the Pt-supported cathode and for the bare Pt foil [Figure 9b(ii)] to ensure that the observed weight difference could be solely ascribed to N2 uptake for the cathode.", "The Brunauer–Emmett–Teller (BET) surface area was then calculated from the Pt-subtracted data by fitting the dependence of N2 uptake with pressure to the BET equation24 in the low pressure range [Figure 9b(iii)].", "For full details of the subtractive technique, BET calculations, and BET surface area results for the tested cathodes, see Supporting Information section S10.4.", "Figure 9 (a) Schematic of the preparation of Pt-supported cathode and subsequent acid removal of the cathode, as used for BET measurements.", "(b) (i) Scheme illustrating the subtractive protocol used to calculate the surface area of the cathodes.", "(ii) Observed weight gain with N2 pressure for a cathode sample of 2 prepared by the method outlined in panel a and for the bare Pt substrate.", "(iii) BET fitting (blue line) for the low-pressure region of N2 sorption data (blue circles) obtained from the difference between as-made Pt supported cathode, 2, and bare Pt substrate.", "This subtractive technique allowed direct determination of the electrode pore volume across the series (Table 2), giving a trend in agreement with the SEM observations (Supporting Information section S10.4 and Figure S17); similar surface areas were observed for all the Mo-substituted systems, which were systematically larger than those found for the Ba0.5Sr0.5(Co0.8Fe0.2)O3−δ parent under the processing conditions used.", "Direct ASR comparisons are thus valid within the Mo-substituted series.", "Table 2 BET Parameters and Derived Surface Areas of the Printed Cathodes from the Point-by-Point Subtractive Techniquea sample C Vm (mmol·g–1) BET (m2·g–1) BSCF 996.0 7.200 × 10–3 ± 5.770 × 10–4 0.70 ± 0.06 1 18.5 3.270 × 10–2 ± 7.730 × 10–4 3.19 ± 0.08 2 23.9 3.261 × 10–2 ± 1.870 × 10–4 3.18 ± 0.02 4 37.7 3.098 × 10–2 ± 6.790 × 10–4 3.02 ± 0.07 aC is the BET constant and Vm is the monolayer adsorbed gas quantity.", "Evolution of the ASR with increasing Mo content z at the Co/Fe ratio m = 4 is nonmonotonic (Figure 8b), although the total DC conductivity σDC (Figure 8c and Supporting Information section S11) decreases as expected from the reduction in d electron and oxygen vacancy concentration on substitution of dn by d0 Mo6+ cations.", "This suggests that Mo catalyzes the oxygen reduction reaction (ORR), consistent with its role in catalytic systems involving dioxygen activation.", "The ASR of 2 (z = 0.375) is lower than that of both SP [z = 0.125 (1)] and SP/DP (z = 0.2, 0.25) materials with reduced Mo contents.", "It is also lower than that of both z = 0.45 (3) from the SP/DP/BaMoO4 region and lower Fe content m = 10, z = 0.45 (4) in the SP/DP region.", "AC impedance arcs at 650 °C [Figure 10a(i)] show that both SP/DP 2 and SP Ba0.5Sr0.5(Co0.8Fe0.2)O3−δ display similar impedance responses dominated by a Gerischer-type contribution [Figure 10a(ii)], which is colimited by oxygen surface exchange and bulk oxide transport.25 All the other higher ASR Ba0.5Sr0.5(Co0.8–xFe0.2–yMox+y)O3−δ materials display different responses associated with charge transfer (electronic) and mass transport (chemical) processes (detailed discussion can be found in Supporting Information sections S10.6–S10.9).", "These comparisons suggest the superiority of the SP/DP architecture of 2 over the SP-only 1 (despite a lower DC resistance for 1), together with the improved performance of this architecture at 2 in comparison with, for example, 4 (m = 10, z = 0.45).", "The relationship between Mo content (and related factors such as oxygen nonstoichiometry, SP phase fraction, and σDC) and ASR implicates the observed SP/DP intragrain microstructure in the cathode performance.", "The mechanistic similarity between 2 and Ba0.5Sr0.5(Co0.8Fe0.2)O3−δ demonstrated by the impedance responses suggest that this SP/DP assembly can give cathode performance comparable to best-in-class single-phase materials, despite being compositionally dominated by an ionic insulator.", "The self-organization of the endotaxial composite confers higher stability than the single-phase parent and opens up the possibility of further optimization in this family of SOFC cathode materials.", "Figure 10 (a) (i) Electrochemical impedance spectroscopy (EIS) arcs for the compositions given in Figure 8a (with the same color scheme) at 650 °C (arcs have been normalized to 0 on the x-axis to remove the electrolyte contribution): symbols are measured data, and lines are from fitting of equivalent circuit models (ECM; Supporting Information section S10.6 and Figure S19).", "The same electrode processes are identified from the ECM for 2 and BSCF, and differ from those occurring in 1 and 4.", "Composition 4 (m = 10) is shown here, as it has lower ASR than 3 (m = 4), which is shown in Supporting Information Figure S19d.", "(ii) Close-up of the EIS arcs for 1, 2, and BSCF shown in panel i.", "As each cathode was manufactured by the same protocol (milling regime, ink processing, screen printing parameters, and thermal treatment) and displays similar morphology and surface area (Supporting Information section S10.4), differences in the observed arcs and selected ECM are a reflection of differences in the electrochemical properties of each composition.", "HRTEM and XRD studies show the phase assemblage and microstructure were unaffected by preparation of the symmetrical cells (Supporting Information section S10.2 and Figure S15).", "The Gerischer-type half-tear-drop shape is apparent in the AC impedance arcs of 2 and BSCF as the dominant large-resistance arc.", "(b) Schematic representation of oxygen ion (red) and electron (black) transport pathways available in a two-phase endotaxial composite grain of 2.", "The absence of oxygen vacancies makes the DP (blue) a pure electronic conductor, whereas oxygen mobility is possible within the SP and along the SP/DP interfaces.", "The SP/DP/air triple phase boundary of 2 is highlighted as an orange dotted line; this boundary, as well as the surface of the SP MIEC regions, is active in the ORR.", "The microstructure of 2 can be approximated as a coherent endotaxial intergrowth of a pure electronic conductor (DP, with no oxygen vacancy content but noninteger transition-metal valence: active in the ORR in isolation only at the triple phase boundary with electrolyte and air) and a MIEC (SP, with vacancies for oxide transport and ORR active at all interfaces with air) (Figure 10b).", "The pathways for electronic conduction are throughout and between the DP and SP regions, whereas oxide ion transport is restricted to the interconnected SP phase regions and their surfaces, including interfaces with the DP.", "The microstructure of Figure 10b creates a high-surface-area triple phase boundary for O2– formation where the electronically conducting, catalytically active DP meets the MIEC SP and air, with the single AO3−δ network interfaces between SP and DP assisting oxide transfer between them.", "The SP component of 2 is richer in Fe than the global m = 4 composition, and thus expected to be a poorer cathode than m = 4 Ba0.5Sr0.5(Co0.8Fe0.2)O3−δ, on the basis of variation of Ba0.5Sr0.5(Co1–xFex)O3−δ performance with Fe content.26 The presence of 70 wt % DP in 2 would be expected to lead to poor cathode performance due to reduced electronic conductivity and absence of oxygen vacancies.", "This is not the case, however: 30 wt % SP alone is not sufficient to account for the low ASR value of 2, as SP/DP Ba0.5Sr0.5(Co0.8–xFe0.2–yMox+y)O3−δ materials such as m = 3, z = 0.21 [63(2)% SP] with higher SP content have higher ASR (Figure 8a,b).", "This shows that the DP is not a spectator phase and that its high Mo and Co content contributes to the oxygen reduction performance of the nanocomposite 2, whose structure favors synergic interaction of the DP and the oxide ion-conducting SP.", "The functional behavior of 2 suggests that the coherent AO3−δ network can integrate the properties of the distinct SP and DP regions to produce performance from the composite that is superior to that expected from the local component phases in isolation.", "Conclusion Composition 2 has superior cathode performance to the other SP/DP materials evaluated because its interplay of SP/DP ratio, domain sizes, phase compositions, and spatial locations best combines the distinct properties of SP and DP.", "It is stabilized by local separation into compositionally and structurally distinct domains of Fe-rich SP and cation-ordered, anion vacancy-free Mo-rich DP, which are spanned by a single AO3−δ network.", "This microstructure results from a heterogeneous distribution of the three electronically active cations over the B-sites.", "The perovskite structure adapts to the compositional complexity and contraindicated chemistry of the three B-site cations that frustrate the formation of a single phase by this reorganization correlated beyond the unit cell.", "The resulting nanoscale modulation of the B-site occupancy produces the compositionally and structurally distinct endotaxially related phases forming the composite.", "The matching of cation occupancy to the crystal chemical environment that is possible in the two-phase B-site separation within a single AO3−δ network increases the stability of the cubic perovskite with respect to competing structures over that of the single-phase parent material.", "The SP/DP composite performs well as an SOFC cathode, exceeding expectations based on the local compositions of the constituent phases (one of which is not capable of anion transport).", "The stability of the self-organized endotaxial composite is thus determined by the local phase compositions, but its properties surpass the sum of these local components in isolation because of the synergic integration of the functions of the two phases by the coherent interfaces of the composite.", "The chemical frustration produced by charge and bonding differences drives the self-assembly of compositionally and structurally ordered regions, spanned by a common network.", "This frustration-based approach is clearly well-suited to the diverse cation ordering patterns known in perovskites.27 The single sublattice phase separation and resulting property integration may also prove applicable to the many well-known families of complex oxides that feature separate structural networks.", "Supporting Information Available Additional text, 11 tables, and 22 figures with information on synthesis methods, analysis of powder diffraction data, Mössbauer spectroscopy, iodometric titration, thermogravimetric analysis, transmission electron microscopy, thermal stability, and electrochemical testing.", "This material is available free of charge via the Internet at http://pubs.acs.org." ]

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[ "A Review of RedOx Cycling of Solid Oxide Fuel Cells Anode A Review of RedOx Cycling of Solid Oxide Fuel Cells Anode FaesAntonin1*Hessler-WyserAïcha2ZrydAmédée1Van HerleJan3 1Design & Materials Unit (UDM), University of Applied Sciences Western Switzerland (HES-SO Valais), Sion 1950, Switzerland; Email: amedee.zryd@hevs.ch 2Interdisciplinary Centre for Electron Microscopy (CIME), Ecole Polytechnique Fédérale de Lausanne (EPFL), Lausanne 1015, Switzerland; Email: aicha.hessler@epfl.ch 3Industrial Energy Systems Laboratory (LENI), EPFL, Lausanne 1015, Switzerland; Email: jan.vanherle@epfl.ch * Author to whom correspondence should be addressed; Email: antonin.faes@a3.epfl.ch; Tel.: +41-27-606-88-31; Fax: +41-27-606-88-15.", "Solid oxide fuel cells are able to convert fuels, including hydrocarbons, to electricity with an unbeatable efficiency even for small systems.", "One of the main limitations for long-term utilization is the reduction-oxidation cycling (RedOx cycles) of the nickel-based anodes.", "This paper will review the effects and parameters influencing RedOx cycles of the Ni-ceramic anode.", "Second, solutions for RedOx instability are reviewed in the patent and open scientific literature.", "The solutions are described from the point of view of the system, stack design, cell design, new materials and microstructure optimization.", "Finally, a brief synthesis on RedOx cycling of Ni-based anode supports for standard and optimized microstructures is depicted.", "SOFC anode RedOx cycle nickel reduction and oxidation reoxidation instability solid oxide fuel cell durability.", "Content Introduction RedOx instability 2.1.", "Problematic 2.2.", "High Temperature Nickel Oxide Reduction and Nickel Oxidation 2.2.1.", "Reduction of NiO 2.2.2.", "High Temperature Oxidation of Ni 2.3.", "Reduction of NiO-YSZ Cermet 2.4.", "Oxidation of Ni-Ceramics Composite 2.4.1.", "Kinetics of Oxidation 2.4.2.", "Homogeneous Versus Inhomogeneous Oxidation 2.4.3.", "Expansion during Reoxidation 2.4.4.", "Bending and Stresses in Half-Cell Samples (Anode Support) 2.4.5.", "Young’s Modulus and Strength Variation with Reoxidation 2.4.6.", "RedOx Expansion Limits: Mathematical Approaches 2.4.7.", "Electrical Conductivity versus RedOx Cycles 2.4.8.", "Temperature Variation during Oxidation 2.4.9.", "Reoxidation by Ionic Current 2.4.10.", "Micro and Nano-Structural Changes upon Redox Cycling 2.4.11.", "Electrochemical Performance and Electrochemical Impedance Spectroscopy 2.4.12.", "Single Chamber SOFC 2.5.", "Summary of the RedOx Instability RedOx Solutions 3.1.", "System Solutions 3.1.1.", "Dependent System Solutions 3.1.2.", "Passive System Solutions 3.1.3.", "Active System Solutions 3.2.", "Stack Design 3.2.1.", "Planar Design 3.2.2.", "Tubular Design 3.3.", "Cell Design 3.3.1.", "Cathode Supported Cell (CSC) 3.3.2.", "Electrolyte Supported Cell (ESC) 3.3.3.", "Metal Supported Cell (MSC) 3.3.4.", "Inert Substrate Supported Cells (ISSC) 3.3.5.", "Anode Supported Cell (ASC) 3.4.", "Modification of the Microstructure 3.4.1.", "Anode Functional Layer, Anode Support and Anode Current Collecting Layer 3.4.2.", "Particles Size 3.4.3.", "Sintering Temperature 3.4.4.", "Porosity 3.4.5.", "Composition 3.4.6.", "Orientation and Particle Shape of Nickel Phase 3.4.7.", "Ni coated Pore-Former 3.4.8.", "Ni Foam 3.4.9.", "Wet Impregnation (WI) 3.4.10.", "Ni Coated Ceramic 3.4.11.", "Graded Composition and Porosity 3.4.12.", "Controlled RedOx Cycle 3.5.", "Alternative Anode Materials 3.5.1.", "Alloys and Additives for Metal-Ceramic Anode 3.5.2.", "Full Ceramic Anode 3.5.3.", "Mechanically Stronger Materials 3.5.4.", "Use Support with Higher Thermal Expansion Coefficient (TEC) 3.6.", "Kinetics 3.6.1.", "Oxidation Barrier 3.6.2.", "Improved Sealing 3.6.3.", "Lower Operating Temperature Synthesis for Ni-Based Anode-Supported Cells Conclusions Acknowledgments Appendix References 1.", "Introduction Fuel cells will play a key role in the future as (1) they convert fuel to electricity with high efficiency (>60%) even for small systems; (2) in electrolyzer mode, they can produce hydrogen from electricity and water to store energy; (3) they are clean (negligible NOx and SOx emissions) and (4) they are silent.", "Solid oxide fuel cells (SOFCs) are based on a ceramic electrolyte and work at elevated temperature between 600 and 1000 °C.", "Their advantages are (1) design flexibility thanks to the solid electrolyte; (2) fuel flexibility including hydrogen, hydrocarbons and bio-fuels and (3) co-generation of heat and electricity (reaching total efficiencies up to 95%) [1].", "Patented in the 1970s, the state-of-the art anode is based on a nickel-ceramic composite material due to its high activity, electrical conductivity and relatively low cost [2].", "The goals of the ionically conducting ceramic are, first, to limit nickel agglomeration at high temperature, second to increase the active electrode thickness and finally to match the anode thermal expansion coefficient (TEC) to that of the ceramic electrolyte.", "The most used ceramics are yttria stabilized zirconia (YSZ) and gadolinia doped ceria (GDC).", "During its fabrication, the anode is sintered at elevated temperature (1300–1450 °C), producing a NiO-ceramic composite.", "The first anode utilization reduces the nickel oxide and creates a porous structure due to the volume reduction from NiO to Ni.", "Majors limitations of the Ni-ceramic anodes are (1) the nickel microstructural changes to lower the interfacial energy, which decreases the electrochemical activity [3,4,5]; (2) the volatilization of the nickel under high steam concentration [6,7]; (3) promotion of the competitive catalytic cracking of hydrocarbons that produces a rapid deposition of carbon in the anode [8]; (4) impurities in the fuel stream, particularly sulfur and phosphorus, that inhibit anode functionality [9] and (5) anode expansion during re-oxidation of the Ni if a fuel supply cut occurs, under high fuel utilization operation or with seal leakage occurrence [10,11,12,13].", "Nickel is not stable, at high temperature, against oxidation in air.", "The volume changes during successive reduction and reoxidation cycles (“RedOx cycle”) may be detrimental for the anode unity.", "The problem is even worse if the cell design is anode supported because the volume change puts the electrolyte under tension and, once cracked, produces leakage between fuel and oxidant gases [10].", "During the last 15 years, a large amount of work has been carried out on the RedOx problematics of SOFC anodes, including three review papers (two considering Ni-YSZ anodes [12,14] and one focused on ceramic anodes [15]), about 10 PhD theses [16,17,18,19,20,21,22,23,24], tens of patents and hundreds of scientific papers.", "This review will try to be as exhaustive as possible.", "It describes first the reduction and oxidation of nickel at high temperature, then continues with the reduction and oxidation of Ni-based composites.", "The effects of RedOx cycles on ceramic-metal (cermet) anode properties, like conductivity, electrochemical performance, dimension, etc., are reported.", "Finally, it reviews the solutions at system, design and materials levels.", "A brief synthesis precedes the conclusion. 2.", "RedOx Instability 2.1.", "Problematic RedOx instability refers to the chemo-mechanical instability of the solid oxide fuel cell anode and support under oxygen partial pressure variation of more than 20 orders of magnitude during reduction and oxidation (pO2,air = 0.21 atm and pH2,3%H2O,800°C = 4 × 10−22 atm) at high temperature (600–1000 °C).", "This was first reported in 1996 by Cassidy et al. for Ni-YSZ anode supported thin electrolyte cells [10].", "The volume increase upon reduction and reoxidation (“RedOx cycle”) of the anode support was measured as well as the loss of the open circuit voltage (OCV) due to cracking of the thin electrolyte.", "This pointed out one of the main limitations of the nickel-ceramic based anode.", "These anodes show a large bulk volume change upon Ni reoxidation.", "The shrinkage of nickel oxide particles during reduction is around 40 vol %, and during reoxidation nickel expansion is around 66 vol %.", "The molar volumes of NiO and Ni are given in Table 1.", "The ratio of molar volume of the oxide and the metal is known as the Pilling–Bedworth ratio and is about 1.66 for nickel [25].", "Based on Cassidy’s and following works, Klemensø drew a schematic of the mechanisms underlying the anode RedOx, as shown in Figure 1 [26,27,28]. membranes-02-00585-t001_Table 1 Table 1 Nickel and nickel oxide molar mass, specific mass and molar volume [29,30].", "NiO Ni M [g/mol] 74.71 58.71 ρ [g/cm3] 6.67 8.9 V [cm3/mol] 10.97 6.58 Figure 1 Microstructural changes during a RedOx process in Ni-YSZ (yttria stabilized zirconia) based anodes [27].", "Anode reduction increases porosity because of the NiO to Ni volume change.", "During utilization, the metallic nickel phase re-organizes due to high temperature, water vapor content and surface tension equilibrium [3,31,32].", "If the oxygen partial pressure increases, nickel can rapidly oxidize at high temperature (above 600 °C).", "The ensuing volume increase can then destroy the electrolyte and the anode support.", "Reoxidation of Ni can occur for a variety of reasons at the operating temperature: Under high load or high fuel utilization conditions, the oxygen partial pressure can locally increase up to a critical value [33]; The oxygen partial pressure increases in the vicinity of compressive seals, which causes small air leakage to the anode [34]; Accidental fuel supply interruption; To reduce cost and system complexity, shut down and start up is done without protective gas.", "This limitation of the state-of-the-art Ni-YSZ anode induced a large research effort from the scientific community as it is considered as one of the bottlenecks of SOFC technology [35].", "Before considering the composite, the reduction and oxidation of pure nickel is discussed. 2.2.", "High Temperature Nickel Oxide Reduction and Nickel Oxidation 2.2.1.", "Reduction of NiO The reduction of NiO occurs by H2 supply and H2O removal according to Equation (1).", "The kinetics of NiO reduction in H2 are commonly approximated by a linear equation with time at constant temperature (Equation (2)), implying a surface controlled process [36].", "Usually the slope is taken at a certain conversion degree (x between 20% and 80%) and its logarithm reported against T−1 to obtain an activation energy (Ea), as the reaction is thermally activated and follows an Arrhenius law (Equation (3)).", "Deviation of linear kinetics at low conversion degree is due to an initial induction period for nucleation of Ni clusters, which then grow at a linear rate.", "At the end of the reaction, it slows down as the diffusion path for H2 reactant and H2O product gets longer through the porous Ni metallic layer.", "This will thus give an “s”-shape curve at low temperature; at high temperature, the induction period is short and the densification of Ni at the surface decreases the gas diffusion process further.", "This is a reason for lower activation energy reported at higher temperature (see Table 2).", "Richardson et al. presented a good description of NiO reduction by hydrogen [37].", "More generally, there are multiple reaction rate equations describing the reduction of metals like a power law, Avrami kinetics or first order kinetics [37,38]. (1) (2) (3) with x the degree of conversion, k the reaction rate, t the time, k0 the reaction rate constant, Ea the activation energy, R the gas constant (8.314 J mol−1 K−1) and T the temperature. membranes-02-00585-t002_Table 2 Table 2 Reduction kinetics for NiO with H2 from Richardson et al. [37] and other authors.", "Source reference Sample and measurement technique Temperature range (°C) Ea (kJ mol−1) Pure nickel oxide Szekely and Evans [37] Large porous single pellet, TGA 372–753 17 Deb Roy and Abraham [37] Non-porous spherical pellets, TGA 400–800 22 Bandrowski et al. [37] Large porous NiO pellet in a packed bed, H2O detection 261–298 52 Szekely and Evans [37] Large porous NiO pellet, TGA 226–308 65 Nakajima et al. [37] Powdered NiO sample 277–377 69 Rao and Rashed [39] Thin NiO slab, TGA 300–400 73 Richardson et al. [37] Porous NiO powder, TGA 220–355 84 Richardson et al. [37] Porous NiO powder thin slab, XRD 175–300 85 Szekely et al. [37] Pressed thin discs, TGA 224–259 133 NiO and ceramic composite Modena et al. [40] Tape-cast NiO-YSZ, TGA 700–800 25–29 Modena et al. [40] Tape-cast NiO-YSZ 2nd reduction, TGA 700–800 51–87 Waldbillig et al. [41] Tape-cast NiO-YSZ, TGA 500–950 54–78 Tikekar et al. [36] Pressed NiO-YSZ rectangular bar, thickness of reduced layer 600–800 94 Pihlatie et al. [38] Tape-cast NiO-YSZ, TGA 500–750 84 Both nickel and its oxide have a face-centered cubic (FCC) structure with the respective lattice parameters equal to 0.368 and 0.418 nm.", "Nickel growth is epitaxial on NiO even if the difference in lattice parameter is 13.6% [42,43].", "The reduction rate is fairly high: at 600 °C a 0.5 mm NiO particle is reduced in 30 min (32% H2 in N2).", "At higher temperature, the kinetics become distorted by sintering of the porous Ni, which limits the access of gas to the oxide [44].", "Addition of water vapor to hydrogen reduces the reduction rate and increases the activation energy at low temperature 175–300 °C for relatively coarse particles (10–20 μm) (for 20% H2 in N2) [37].", "Contradictorily, Müller relates that if the water vapor is increased from 3% to 10%, the reduction temperature decreases and the rate increases for fine NiO particles of 0.5 μm (for 6% H2 in N2) [16]. 2.2.2.", "High Temperature Oxidation of Ni This section is based on three different books [25,45,46] and a review paper from Atkinson [47] describing high temperature oxidation of metals.", "The oxidation forms on top of the metal an oxide layer that separates the gas containing the oxidant species and the metal.", "In case of nickel, the reaction occurring in air is Ni + 1⁄2O2 = NiO.", "For a thin oxide layer (< about 0.1 μm), transport is governed by the electric field built within the layer by the cathodic reaction (1⁄2O2 + 2e− = O2−) and the anodic one (Ni = Ni2+ + 2e−).", "This oxidation rate is described by the Mott–Cabrera theory and follows logarithmic laws.", "For thicker oxide layers (>0.1 μm), oxidation is governed by ion diffusion through the oxide scale, which follows a parabolic behavior (Wagner theory), with y2 = kp·t, where y is the oxide layer thickness, t the time and kp the parabolic rate constant.", "The Ni2+ cation diffusion in its oxide is about 6 orders of magnitude faster than the oxygen anion diffusion at 1400 °C.", "This can cause internal voids during the growth of the oxide layer.", "For large surfaces, the inward diffusion of oxygen occurs through microcracking or microchannel formation.", "The microstructure of the oxide surface and cross-section varies depending on the oxide thickness and the oxidation temperature as shown by Peraldi et al.", "(see Figure 2) [48,49].", "Figure 2 Arrhenius plot of parabolic rate constant kp as a function of oxidation temperature and scale thickness indicating NiO scale morphologies and microstructures [48,49].", "In the case of small metal particles, it was observed by focused ion beam cross-sectioning that internal porosity is formed due to different diffusion coefficients between Ni2+ and O2− in the nickelous oxide like a pseudo Kirkendall effect (a pure Kirkendall effect is for a metal solid solution; in the case of NiO, Ni2+ and O2− are on different crystallographic positions).", "Up to 1000 °C, outward diffusion of nickel cations is faster than the inward diffusion of oxygen anions, leaving NiO internal porosity [50].", "For metal nanoparticles, the number of voids and the void’s growth depend on the relative rate of self-diffusion in the core material (i.e., Ni or vacancy diffusion in Ni crystal) versus cation diffusion through the shell (i.e., Ni2+ diffusion in NiO crystal) [51].", "If self-diffusion is fast, a single void may form inside the particle and grow until conversion is completed (e.g., NiO).", "Alternatively, if self-diffusion is significantly slower than cation diffusion through the oxide shell, then several voids remain (e.g., CoO and CoxSy) [52].", "For the Ni case, the particle size plays a role: smaller nanoparticles show single voids compared to larger nanoparticles presenting multiple voids.", "For the larger nanoparticles, the Ni self-diffusion is not fast enough to condense all the vacancies into a single void [53].", "The key factor in microstructural modification during oxidation is the difference in diffusion coefficients defining the mass transport.", "By decreasing the oxygen partial pressure, the oxidation rate should decrease proportionally to kp = C × (pO2)1/6 (with C a constant).", "The equilibrium partial pressure of oxygen can be calculated using the Gibbs free energy of the nickel oxidation reaction (Ni + 1⁄2 O2 ↔ NiO).", "From this a Nernst potential can be calculated against an electrode in air depending on the temperature: (4) where T is the temperature in Kelvin, R the gas constant, F the Faraday constant and pO2cathode the partial pressure of oxygen at the cathode side.", "The value of the Nernst potential (or open circuit potential, OCV) versus temperature during Ni oxidation is given in Figure 3: at 800 °C, the OCV is between 0.68 and 0.71 V depending on the chosen database for the Gibbs free energy [54,55].", "Figure 3 Open circuit voltage (OCV) or Nernst potential versus temperature for the Ni/NiO equilibrium [54,55].", "Solid state diffusion is activated by temperature as expressed by the Arrhenius Equation (3).", "Values of the activation energy are given in Table 3.", "It is observed that the rate at low temperature is higher than predicted by the exponential approach.", "At low temperature, the metal ions diffuse through the NiO grain boundaries and linear defects (dislocation and twins).", "Thus the oxidation rate will depend on the grain size in the oxide layer [47]: (5) where g is the grain size, D* the diffusion coefficient of Ni2+ in the NiO lattice, D' the diffusion coefficient of Ni2+ at the NiO grain boundaries and δ the thickness of the NiO grain boundaries (about 1 nm).", "Alloying the nickel increases the oxidation rate constant (see Figure 4).", "If the alloying element concentration is high enough to form a dense protective layer, the rate constant decreases (see Si and Cr in Figure 4).", "The simultaneous addition of two alloying elements can form a stable oxide layer at lower overall weight concentration than a single element (see Figure 5). membranes-02-00585-t003_Table 3 Table 3 Oxidation kinetics of nickel and nickel cermet in air (with Ø for particle diameter).", "Source Reference Sample Temperature range (°C) Ea (kJ mol−1) Kinetics Pure nickel Suwanwatana et al. [56] Ni particles, Ø = 79 nm 250–350 150 Deviation from parabolic Suwanwatana et al. [56] Ni particles, Ø = 0.7 μm 250–350 127 Deviation from parabolic Suwanwatana et al. [56] Ni particles, Ø = 3 μm 250–350 108 Deviation from parabolic Karmhag et al. [57] Ni particles, Ø = 15 nm 135–235 129 Deviation from parabolic Karmhag et al. [58] Ni particles, Ø = 5 μm 300–700 145 Deviation from parabolic Karmhag et al. [59] Ni particles, Ø = 158 μm 500–700 183 Deviation from parabolic Haugsrud [60] Polycrystalline Ni-mechanically polished 500–800 150 Deviation from parabolic Karmhag et al. [59] Ni particles, Ø = 158 μm 800–1200 116 Deviation from parabolic Haugsrud [60] Polycrystalline Ni-mechanically polished 1100–1300 200 Parabolic Peraldi et al. [61] Polycrystalline bulk Ni-mechanically polished 1000–1200 200 Parabolic Nickel–ceramic composite Waldbillig et al. [41] Tape-cast NiO-YSZ 500–850 87–92 Deviation from parabolic Tikekar et al. [36] Pressed NiO-YSZ rectangular bar 600–800 – Parabolic Stathis et al. [62] Warm pressed NiO-YSZ 550–650 Logarithmic Modena et al. [40] Tape-cast NiO-YSZ 700–800 37–44 Logarithmic Pihlatie et al. [38] Tape-cast NiO-YSZ 500–1000 Linear–parabolic–logarithmic part Roche et al. [41] Tape-cast NiO-YSZ 600–1000 118 Deviation from parabolic Czerwinski et al. [63] Polycristalline Ni with CeO2-mechanically polished 600–800 88 – Czerwinski et al. [63] Polycristalline Ni with CeO2-chemically polished 600–800 100 – Galinski et al. [64] Thin sprayed NiO-40CGO 500–575 164 Parabolic–cubic Galinski et al. [65] Thin sprayed NiO-CGO 500–575 270 Mott–Cabrera equation for spherical geometries Figure 4 Effect of alloying on the rate constant for oxidation of nickel in air at 900 °C [46].", "Figure 5 Oxide map for alloys in the Ni-Cr-Al system delineating the composition ranges for formation of different types of oxide scales [25]. 2.3.", "Reduction of NiO-YSZ Cermet The composite structure of the as-sintered NiO-YSZ anode changes the behavior during reduction and re-oxidation, compared to pure Ni/NiO.", "Comparison of the reduction behavior of original NiO powder and NiO-YSZ anode during heating under reducing atmosphere in a thermogravimetric analyzer (TGA) shows a higher starting temperature and a slower rate for the composite structure [66].", "By contrast, in situ transmission electron microscopy (TEM) shows a NiO-reduction starting at the NiO-YSZ interface.", "This contradictory result may come from the lower hydrogen pressure in the TEM and the different surface defects between TEM and bulk samples [67].", "Tikekar et al. performed reduction on dense NiO-YSZ fabricated by compaction and measured the reduction rate by measuring the reduced layer thickness versus time.", "They found linear kinetics with an activation energy of 94 kJ/mol [36].", "Waldbillig et al. performed reduction of tape-cast samples in a TGA and measured the activation energy (Ea) by constant heating rate and constant temperature reduction and found a similar activation energy as for NiO powder, showing that the gas diffusion in NiO-YSZ dense samples is not limiting the kinetics (see Table 1) [41].", "Pihlatie et al. observed also linear kinetics up to 80% NiO conversion with similar Ea (between 500 and 750 °C) [38].", "At high temperature (between 750 and 1000 °C), they reported a small decrease in the reduction rate by adding 3% water vapor to 9% H2 in N2 and attributed it to coarsening of the Ni phase under water vapor.", "Grahl-Madsen et al. observed an increase in electrical conductivity by increasing the temperature of reduction [68].", "The high conductivity could not be obtained by increasing the temperature after an initial reduction at lower temperature.", "This shows that the Ni phase is highly mobile during reduction of NiO.", "Li et al. measured the performance of anode-supported cells against temperature of reduction (between 550 and 750 °C) and found for their case an optimal reduction temperature for 650 °C [69].", "Jung et al. proposed to carry out the reduction via the ionic current (applying external potential to drive the O2− from the NiO based electrode through the electrolyte) to enhance cell performance [70].", "Pihlatie et al. observed a transient shrinkage (0.08%) of the composite sample during reduction at lower temperature (600 °C), which is due to the contraction of NiO to Ni [38,71].", "At higher temperature the stress in the Ni phase is released by creep.", "The shrinkage of the Ni-YSZ composite depends on the temperature, with 0.04%, 0%, 0.01%, 0.05% and 0.3% of shrinkage after 15 h of reduction at 600, 750, 850, 1000 and 1100 °C, respectively [72].", "It also depends on the as-sintered porosity of the sample: no shrinkage was noted up to 14% porosity, but 24% and 33% porosity led to 0.01% and 0.03% of shrinkage after 10 h of reduction at 850 °C, respectively [73].", "The sample composition plays a big role: coarse NiO and YSZ powders could show up to 2.1% shrinkage after 25 h at 850 °C, while the addition of 20% of fine YSZ reduced the shrinkage to 0.5% for the same conditions [68].", "Multiple RedOx cycles lead to a faster reduction rate after the first reoxidation [27,74,75].", "This is due to the opening of the microstructure by breaking the thin electrolyte and the YSZ backbone and the change in the nickel oxide nano- and micro-structure.", "This will be described in more detail in the next section.", "Temperature programmed reduction showed that reoxidized NiO re-reduced at lower temperature than before the reoxidation, confirming the change in NiO nanostructure [76]. 2.4.", "Oxidation of Ni-Ceramics Composite This section reports observations during oxidation of the Ni-YSZ composite as described in the literature.", "The nomenclature introduced by Ettler et al. includes “external parameters”, like temperature, incident oxidant flow, duration of oxidation and gas flow rate, versus “internal parameters”, which are linked to the Ni-YSZ design, microstructure and composition [77].", "This section will discuss the external parameters. 2.4.1.", "Kinetics of Oxidation In comparison to pure Ni (reduced in similar conditions), the composite starts to oxidize at lower temperature and with a faster rate [66].", "An early study on in situ reduction of NiO-YSZ in a X-ray diffractometer showed that isothermal reoxidation at 600 °C is faster than the reduction at the same temperature [78].", "The study of the oxidized layer thickness vs. time showed a parabolic behavior during re-oxidation of Ni-YSZ, indicating a diffusion-controlled process.", "As this process is not thermally activated, the conclusion is that the limiting rate is the diffusion of oxygen gas through the oxidized layer with an effective diffusion coefficient of 10−7 cm2/s [36].", "A TGA study observed a parabolic behavior at low temperature (400–650 °C) and a divergence from parabolic behavior between 700 and 850 °C, the activation energy being lower than the usual values observed for pure Ni (see Table 2) [41].", "Other studies show logarithmic behavior of the oxidation of Ni-YSZ cermet activated by temperature at 550–650 °C [62] and 700–800 °C [40].", "The difference in these results could come from the fact that the limiting process changes from solid state diffusion at lower temperature to gas phase diffusion at higher temperature, due to pore closing when Ni changes to NiO at the composite surface.", "The ideal-gas law gives a diffusion coefficient proportional to T3/2 [79] (high temperature cermet oxidation), compared to solid-state diffusion following the Arrhenius law (proportional to exp(−Ea/RT), for low temperature cermet oxidation).", "Pihlatie et al. show a change in activation energy around 750 °C [38], whereas Roche et al. observe this transition around 800 °C in 20% O2.", "At lower pO2, the transition occurs at a lower temperature: with 1% O2, the gas diffusion is limiting the oxidation down to 600 °C [80].", "The porosity of the support plays a role in the oxidation kinetics and makes the direct comparison of the different studies problematic, due to their different microstructures.", "Kinetics of oxidation of a Ni-Gd0.4Ce0.6O2 (40CGO) anode was studied by in situ X-ray diffraction between 500 and 575 °C, where a transition between parabolic to cubic behavior was observed.", "The time for full oxidation of nickel in the anode is 4 min at 650 °C and only 0.5 s at 850 °C [64] (the anode thickness was not given but it can be estimated to around 25 μm from a parallel study [81]).", "A following study fitted the oxidation kinetics between 500 and 575 °C of Ni-CGO composite with a Mott–Cabrera equation for spherical geometries.", "The higher activation energy compared to other studies (see Table 3) should be related to the compressive stress built up in the composite [65].", "Multiple RedOx cycles showed a faster rate for the second reduction and second oxidation [27,74,75].", "This is closely related to the faster reduction process: higher gas diffusion in the more open microstructure due to cracks in the YSZ electrolyte and skeleton, and finer Ni grains after the first cycle, as the oxidation is inversely related to the grain size (see Equation (5)).", "A temperature programmed oxidation study also revealed a finer Ni microstructure after a RedOx cycle [82]. 2.4.2.", "Homogeneous Versus Inhomogeneous Oxidation The change in cermet oxidation kinetics with temperature can be linked to the transition from “homogeneous” to “inhomogeneous” oxidation.", "The first observation of homogeneous oxidation appears at low temperature (550–650 °C) under dry air where the full anode layer starts to oxidize homogeneously.", "By comparison, between 900 and 950 °C under Ar with 40% to 80% water vapor, oxidation starts at the surface and then moves inward with time.", "In inhomogeneous oxidation, a sharp border between oxidized and reduced side of the sample can be observed.", "This inhomogeneous oxidation leads to a warping or bending of the composite sample [62].", "Further studies showed that oxidation under air between 700 and 800 °C also presented “inhomogeneity” and bending of the samples, compared to lower temperature oxidation (600 °C) [14,77,83].", "At low temperature, oxidation kinetics is limited by the diffusion in solid state.", "At higher temperature, the limitation comes from gas diffusion through the re-oxidized layer, which has high tortuosity and low porosity.", "These observations can be compared to the results from Tikekar et al. [36], where they measured the thickness of the oxidized layer in air versus time, down to a temperature of 650 °C.", "Intrinsically, the sample oxidation has to be inhomogeneous in order to perform the measurement of oxidized layer thickness versus time.", "Only the gas limitation kinetics can be observed using this technique.", "Therefore Tikekar et al. did not observe thermally activated oxidation [36].", "As mentioned before, the ideal gas law gives a diffusion coefficient proportional to T3/2 [79] compared to solid-state diffusion following the Arrhenius law (proportional to exp(−Ea/RT)).", "This can be related to the kinetics of the reaction: inhomogeneous oxidation corresponds to O2 gas diffusion limited oxidation (high temperature and low pO2) and homogeneous oxidation is related to solid state diffusion limitation (low temperature and high pO2).", "Some authors observed oxidation inhomogeneity at 650 °C [36] and others only from 750 °C [14].", "This is probably related to the cermet microstructure: Lower porosity samples show inhomogeneous oxidation and bending at lower temperature.", "By lowering the partial pressure of oxygen of the oxidizing flow (from 50% to 20% and to 0.1% in He), the inhomogeneity of oxidation (and the sample bending) increased [83,84]. 2.4.3.", "Expansion during Reoxidation The volume expansion of the anode due to nickel oxidation creates stresses in the different layers (compression in the anode and tension in the electrolyte).", "The stresses are proportional to the expansion: an essential measurement for the anode RedOx stability is dilatometry during re-oxidation.", "Theoretically, an expansion higher than 0.2% will fracture the thin electrolyte in case of an anode supported cell (see Section 2.4.6 for more details) [12,85].", "Expansion was also measured at room temperature after re-oxidation [76,86] but the TEC variation between NiO-YSZ and Ni-YSZ composite should be taken into account [87]; the maximal strain can occur during oxidation and not after completion [88].", "Dilatometry was performed in situ during oxidation at the initial stage of Ni-YSZ studies [62,89,90].", "In 1998, Mori et al. reported an important expansion during TEC measurement of a 35 vol % Ni-YSZ sample in air [87]: At around 900 °C the expansion strongly increased, by about 1.2% to 1.5%.", "They observed cracks at the 8YSZ grain boundaries.", "Stathis et al. observed an increase in expansion with oxidation temperature in air, from 0.27% to 0.54% at 650 and 800 °C, respectively [62].", "This is confirmed by other authors: Pihlatie et al. observed an expansion from 0.19% to 0.28% and to 0.93% at 600, 800 and 1000 °C, respectively [72].", "Klemensø et al. saw even much higher expansion, from 0.99% to 4.95% at 700 and 1000 °C, respectively [26].", "The difference in expansion for similar conditions could be related to a difference in microstructure, as shown by Fouquet et al. [66] and Waldbillig et al. [41].", "This will be discussed in more detail in the next section.", "The effect of nickel sintering in reducing atmosphere on the expansion during a RedOx cycle was confirmed by Pihlatie et al., who found a doubling of the expansion for a sample reduced for 4.5 h at 1100 °C, compared to a sample reduced for 5.5 h at 800 °C [72].", "This confirms the suggestion proposed by Cassidy et al. in 1996 [10] and presented in the small model (Figure 1) shown by Klemensø et al. about ten years later [26].", "The water vapor plays an important role also during reoxidation as shown by the increase of expansion from 0.68% to 0.96% at 850 °C under dry air resp. air with 6% H2O, though at 600 °C no difference was observed.", "The effect of humidity at 850 °C is similar to the effect of increasing temperature up to 1000 °C [72].", "This is an important result as at high fuel utilization, the water vapor on the anode side can reach high values depending on the fuel (up to 80%–90% under pure hydrogen).", "Then reoxidation will occur under high water vapor concentration.", "A small expansion at 850 °C was observed at an oxygen partial pressure of 5 × 10−12 atm, which is about 50 times the equilibrium partial pressure of oxygen for the Ni/NiO couple at this temperature [72].", "Usually, subsequent RedOx cycles present an irreversible behavior as the contraction is smaller than the expansion; the second oxidation therefore reaches a higher maximal cumulative RedOx strain (CRSmax) than during the first oxidation [72].", "This behavior is observed by other authors [26,66,76].", "At lower temperature the behavior can be reversible [76].", "Sarantaridis et al. presented a nearly linear behavior between the oxidation strain and the degree of oxidation (DoO) with a small shrinkage of 0.05% at 5% DoO and a maximum strain of 0.55% reached at a DoO between 90% and 95%.", "The second oxidation presents the same behavior with a shift to a higher strain of about 0.1%.", "They also observed a difference in strain after the first oxidation at 800 °C when the sample was measured at room temperature (i) with interruption during oxidation; (ii) without interruption and (iii) for in situ dilatometry measurement (high temperature).", "Results were 0.55%, 0.65% and 0.80%, respectively [50].", "Another study used crack widths in the thin electrolyte and the porosity increase in the anode for the expansion calculation after multiple RedOx cycles.", "From temperature variation, a “RedOx safe” temperature could be extrapolated downwards to 550 °C for this microstructure at which the thin electrolyte will not crack upon RedOx cycling.", "This was confirmed experimentally, also for real stacks experiencing fuel supply interruption.", "Repeated RedOx cycles at 800 °C showed a stabilization of the RedOx strain after multiple cycles [85].", "Based on dilatometry measurements, Pihlatie et al. proposed a model based on continuum mechanics to fit all experimental expansion data versus temperature.", "The simulation shows that during reduction at low temperature (600 °C), the contraction of the sample is due to the limited creep in the nickel at these temperatures.", "During reoxidation at low temperature, the model shows that pseudo-plasticity or micro-cracking occurs in NiO, that at 850 °C the 3 mol % Y2O3-tetragonal zirconia polycrystal (3Y-TZP) backbone fractures and that at 1000 °C the 3Y-TZP creeps and undergoes micro-cracking.", "The main limitations of the model are that (1) the strength of 3Y-TZP is back-calculated and (2) the critical stress for pseudo-plasticity in NiO is directly dependent on the value used for NiO fracture toughness and critical flaws in NiO.", "These unknown parameters basically allow the fit of any RedOx strain [71]. 2.4.4.", "Bending and Stresses in Half-Cell Samples (Anode Support) Stresses in the layers are present due to the difference in thermal expansion coefficient (TEC) between the anode and the electrolyte.", "The TECs for pure 8YSZ, NiO and Ni are 10.3, 14.1 and 16.9 × 10−6 K−1, respectively [87].", "For a standard composition containing 58 wt % NiO, which corresponds to 56 vol % NiO and 43 vol % Ni, the corresponding TEC is 12.3 and 11.5 × 10−6 K−1, for the oxidized and reduced states, respectively [87].", "This means that the electrolyte, which shrinks less during cooling, will be under compression and the anode under tension with a maximal value at the interface with the electrolyte [91].", "The stress and bending calculations were done for CGO-YSZ, by Atkinson and Selçuk, and gave good results with a “stress free” state around 1200 °C [92].", "Stress measurements were done on NiO-YSZ half-cells with a thin 8YSZ electrolyte using X-ray diffraction (XRD) at room temperature: The thin electrolyte stress is about −560 MPa and does not vary when the cell is flattened for stacking.", "The reduction of the half-cell for 10 h at 900 °C reduces the stress by about 10% [91].", "These results are comparable to those reported by Sumi et al. on NiO-3YSZ anode-supports (300 μm) with 10ScSZ electrolyte (20 μm).", "At room temperature, the as-sintered electrolyte stress is −400 MPa, in the reduced state −250 MPa, and −170 MPa in the reoxidized state.", "The thin electrolyte showed cracks after reoxidation.", "The compressive stresses after reoxidation are due to the cooling from the RedOx temperature to room temperature.", "The anode is under tension of 50–100 MPa at the interface with the electrolyte.", "In situ measurements in a high energy (70 keV) X-ray synchrotron beam showed that the stresses are released at 1000 K [91].", "Reasons for the electrolyte internal stress change between reduced and oxidized states are: (1) At high temperature, the porosity increase in the reduced anode lowers its Young modulus [93] and (2) at room temperature, the TEC changes between the oxidized and reduced Ni-YSZ composite [87].", "Another study reported higher compressive stresses measured on NiO-YSZ anode-supports and YSZ electrolyte using a similar XRD technique and microscopic strain in 5 μm electrolyte grains (with an advanced method and synchrotron radiation [94]): The values were −690 MPa, −600 MPa and about 0 MPa, for room temperature as-sintered, reduced and re-oxidized samples, respectively.", "The electrolyte residual stress at 800 °C was measured as −60 MPa [95].", "Tanaka et al. presented the following work of Sumi et al. on similar samples.", "The in situ oxidation of Ni-3YSZ anode-supports during measurement showed a tensile stress in the electrolyte of 150 MPa at 800 K (see Figure 6).", "The Ni peaks disappear between 550 and 650 K when the nickel oxidizes.", "A difference of more than 100 K exists between the Ni peak disappearance and the tensile stress occurance [96].", "The final stress in the electrolyte is similar to the one before the RedOx cycle; the thermal stresses are built up again, in contradiction to the stress release observed by Villanova et al. at room temperature [95].", "When oxidation occurs on one side, the half-cell bends due to chemo-mechanical expansion.", "This was observed in situ during oxidation at 800 °C of a half-cell composed of an anode-support, an active layer and a thin electrolyte of a total thickness of 0.27 mm [97].", "As the oxidation starts at the anode, the cell bends towards the electrolyte (electrolyte on the concave side), then the curvature comes back to its initial value and bends further towards the anode (Figure 7).", "The authors explain the bending towards the electrolyte with an elastic deformation model but such a model cannot explain the bending towards the anode.", "Other authors propose plastic deformation of the anode during reoxidation to describe the anode being on the concave side after RedOx cycles [85,98].", "Figure 6 Changes in stresses in 10ScSZ (scandium-stabilized zirconia) electrolyte and anode during heating Ni-3YSZ under air [96].", "Figure 7 Curvature change during reoxidation and re-reduction cycles (0.27 mm half-cell, 800 °C) [97].", "During re-oxidation, the half-cell shows (i) an initial curvature towards the electrolyte (on the concave side); then (ii) it reverts to “zero”-curvature and finally (iii) it stabilizes with a curvature towards the anode (on the concave side).", "Other studies with NiO anode-supports with a 10CGO (10 mol % gadolinia-doped ceria) thin electrolyte showed bending with the anode on the concave side after reoxidation at 750 °C [99].", "Ettler et al. showed that their NiO-YSZ (half-cell and full cell) bending towards the anode occurs at oxidation temperature higher than 700 °C, but that at lower temperature the bending is towards the electrolyte.", "They conclude that inhomogeneous oxidation bends the half-cell towards the anode (on the concave side, as shown in Figure 7) and homogeneous oxidation does the opposite [14].", "Another in situ study revealed a curvature towards the electrolyte after re-oxidation at 800 °C [100].", "By lowering the partial pressure of oxygen during reoxidation of a half-cell (at a constant temperature), the bending towards the anode is increased [83,84].", "Half-cell samples with low porosity bent towards the anode (on the concave side) after 5 RedOx cycles at 750 °C, compared to higher porosity samples that stayed flat.", "The crack density in the thin electrolyte was higher in the case of the lower porosity samples as shown in Figure 8 [98].", "Figure 8 Picture of Ni-YSZ anode supported half-cell discs after 5 reduction-oxidation cycling (RedOx cycles) at 750 °C.", "(A) and (C): samples with 17.5% as-sintered porosity and (B) and (D): samples with 12% as-sintered porosity.", "The electrolyte is face-down for (A) and (B).", "A clear difference in curvature is observed between the two groups of samples comparing (A) and (B), (B) is bent towards the anode (anode face-up on the concave side).", "A clear difference in crack density is observed between the two groups of samples comparing (C) and (D) [98].", "Laurencin et al. studied the creep of the Ni-YSZ anode under reducing atmosphere.", "In the case of anode-supported cells (ASC), the compressive stresses decrease during the first 500 h of utilization from −220 to −120 MPa (based on creep measurement).", "This means that the RedOx tolerance of the thin electrolyte becomes lower with time as the compressive stresses in the electrolyte “work” against the RedOx anode strain.", "In the case of electrolyte-supported cells (ESC), the creep behavior will be beneficial by preventing the build-up of a high stress level after several RedOx cycles [101]. 2.4.5.", "Young’s Modulus and Strength Variation with Reoxidation Young's modulus, strength and fracture toughness of NiO-YSZ and Ni-YSZ composites are well described by Atkinson and Selçuk [102] and Radoviç and Lara-Curzio [93].", "The general trend is a decrease of the mechanical properties with increasing porosity (models are presented).", "Pihlatie et al. used the impulse excitation technique (EIT) to study the evolution of Young’s modulus of NiO-YSZ with temperature in the as-sintered, reduced and reoxidized states [103].", "They obtained a relation between the RedOx strain and the decrease in Young’s modulus.", "The damages caused by the RedOx cycles degrade the elastic properties.", "It starts linearly from 0.5% to 0.6% redox strain to macroscopic sample failure at 2.5%.", "An isotropic continuum damage model is given to fit the degradation: E = (1 − w) × E0 , with w the damage variable as a function of the oxidation strain (see Figure 9).", "Sarantaridis et al. showed a linear increase of the Young modulus (E) with the degree of oxidation (DoO), starting at 32 GPa and ending at 74 GPa [50].", "The as-sintered E with 79 GPa is higher than for the reoxidized sample.", "The Young modulus is directly linked to the sample porosity [102], therefore the 5 GPa decrease can be related to a total porosity increase from 26.4% before to 27.6% after the RedOx cycle.", "Figure 9 Mechanical degradation in terms of relative loss of elastic modulus of NiO-YSZ composite in its oxidized state during RedOx cycle as a function of the oxidation strain (CRS: cumulative redox strain).", "The measurement is reproducible (i.e., samples 1 and 2) [103].", "Pusz et al. presented NiO-YSZ anode-supported tubular cells with an external diameter of 7.31 mm and a wall thickness of 1.7 mm.", "This study compared the strength evolution with RedOx cycles using ten samples each time of two compositions: (1) A fine structure containing black nickel oxide and (2) a coarse structure based on green NiO (dv,50 = 0.95 μm) with 40:40:20 vol % of NiO:8YSZ:Carbon pore former.", "Strength was measured at room temperature after 1 h RedOx cycling at 800 °C (see Figure 10).", "The strength of the fine microstructure sample doubled after 3 RedOx cycles.", "After the third RedOx cycle, the strength starts to decrease.", "The coarse microstructure showed a decrease in strength after reduction, a small increase for the first RedOx cycle and then a linear decrease with the RedOx cycle number [104].", "Similar results were shown for planar anode supported cells after 10 RedOx cycles at 800 °C using 10 disc samples per measurement (25 mm of diameter).", "The mechanical strength of these supports increased slightly from 145 to 155 MPa after 10 RedOx cycles (the Weibull modulus also increased from 6 to 9) [105].", "Another study on planar Ni-3YSZ half-cells showed no variation on strength after one RedOx cycle at 750 °C [98].", "The authors were not very clear about the increase in strength during RedOx cycles.", "As maximal stress is located at the tube surface and the strength depends on the flaw distribution, this evolution can be linked to the surface change during RedOx cycles: densification of the surface lowers the flaw size at the surface.", "Figure 10 Strength of the C-shaped uniaxial compressed anode rings versus number of RedOx cycles.", "The samples were fabricated using two different powders, coarse green NiO and fine black nickel oxide [104]. 2.4.6.", "RedOx Expansion Limits: Mathematical Approaches Sarantaridis and Atkinson presented an analytical approach based on the release of stored elastic energy under plane strain conditions for modeling the maximal strain of the anode during RedOx cycles in case of anode-supported cells (ASC), electrolyte-supported cells (ESC) and inert substrate or metal-supported cells (MSC) [106].", "The maximal strain of planar ASC before cracking the thin electrolyte can be deduced from Equation (6): (6) with E the Young modulus of the electrolyte, v the Poisson ratio, h the electrolyte thickness, εox the oxidation strain, GASC and Gc the stored and the critical energy release rate, respectively.", "Substituting the typical values given in [106], the product ε2ox hc = 7.4 × 10−12 m is a constant, with hc the critical thickness when GASC = Gc.", "The interesting point is that a decrease in electrolyte thickness increases the RedOx stability (more RedOx strain possible).", "Thus, for a given oxidation strain of 1%, the critical thickness is as small as 0.074 μm.", "An electrolyte thickness of about 2 μm gives a RedOx strain limit of 0.2%.", "In case of elastic relaxation, the crack spacing, l, is given by 8h/ln(h/hc), which means no extensive damage will occur until hc < 2h.", "Hence an electrolyte of 4 μm thickness could be tolerated.", "For the electrolyte-supported configuration, the failure mode will be delamination of the anode.", "Based on 8YSZ with a certain porosity, delamination occurs if the anode exceeds 2.6 μm; for a 10 μm anode, an oxidation strain of 0.5% can be tolerated.", "Buckling of the anode requires an initial delamination of 170 μm in size.", "Decreasing the thickness increases the strain linearly; hence a thin anode layer is more RedOx stable.", "Cracks in the thin electrolyte for ASC configuration (Figure 11) and delamination of the anode for ESC (Figure 12) are shown by other authors confirming the degradation mechanisms proposed by Sarantaridis and Atkinson.", "Figure 11 Thin electrolyte crack formation during two RedOx cycles in the anode supported cell design.", "(a) co-firing; (b) reduced (c) re-oxidized; (d) second reduction; (e) second oxidation and (f) third reduction with an additional 100 h under reducing atmosphere [14,107,108].", "Figure 12 Delamination of anode and anode current collection layer in case of 8YSZ electrolyte supported cells after five RedOx cycles at 950 °C and 40 min.", "Right: Only Ni-8YSZ active anode; left: active anode plus Ni-8YSZ current collecting layer [16].", "For a metal support, in case of edge initiation delamination with a thickness of 10 μm each for the cathode, the electrolyte and the anode layers, a limit of 1% strain can be obtained.", "In summary, the maximum RedOx strain before degradation is: 0.2% for ASC, 0.5% for ESC and 1% for MSC.", "ASC is the most sensitive geometry in terms of RedOx stability, not only because it is breaking the gas tight electrolyte, but also due to the layer configuration.", "Klemensø [27] and Klemensø and Sørensen [109] proposed an approach including anode support (AS), active functional layer (AFL) and electrolyte for the ASC case.", "Usually, the AFL has a finer microstructure to enhance electrochemical performance whereas the AS serves proper mechanical stability, sufficient electrical conductivity and gas transport properties.", "Lowering the temperature and decreasing the anode support thickness will increase the RedOx stability.", "For AS thickness of 300 μm, AFL and electrolyte thickness of 10 μm, the maximal strains before electrolyte cracking are: at 650 °C, 0.2% for AS and 0.7% for AFL; at 800 °C, 0.2% for AS and 0.25% for AFL.", "Based on finite element modeling (FEM) calculations and failure probabilities of a Ni-YSZ anode-supported cell with 1 mm thick support, 10 μm thick 8YSZ electrolyte and 60 μm thick LSM cathode with a cell diameter of 116 mm, it has been shown that the cathode will crack when the support expands by more than 0.05%–0.09% and when the electrolyte expands by more than 0.12%–0.15% (see Figure 13) [110].", "Figure 13 Survival probability of LaSrMn-oxide (LSM) cathode (60 μm) and YSZ electrolyte (10 μm) against the strain of the Ni-YSZ anode support (1 mm) [110].", "Some singularities are considered in the modeling and give hints for the fabrication, e.g., that the cathode/electrolyte contact angle at the cathode side in an ASC should be higher than 90° to increase stability [111].", "The ESC configuration with a 10 μm thick anode will delaminate after 0.3% to 0.35% expansion.", "Experimental results based on the ASC from the Forschungszentrum Jülich (FZJ) showed that the electrolyte cracked after a degree of oxidation between 56% and 70.7% at 800 °C (similar to the value obtained by Sarantaridis et al. [112]), which corresponds to an expansion between 0.26% and 0.34%.", "Modeling underestimated the maximal value of expansion, which could be due to the inhomogeneity of oxidation at 800 °C in that only the anode side opposite to the electrolyte was oxidized.", "Cracks in the electrolyte were quantified by SEM and permeability of the electrolyte and expansion were measured using micro-Vickers marks distance before and after expansion [113].", "Based on Weibull statistics and FEM, it can be seen that sample size influences the maximal anode strain before ACS thin electrolyte cracking, from 0.18% for small samples (0.1 cm2) to 0.12% for total stack surface (2000 cm2) [85].", "Sarantaridis et al. compared the oxidation in air with oxidation by ionic current at 800 °C.", "They proposed a model that takes into account the non-uniformity of the electrochemical reoxidation on the failure probability of the electrolyte.", "The critical degree of ionic current reoxidation occurs at 3% (compared to 49% to 75% by oxidation in air), it creates a compressive stress in the central reoxidized anode located under the cathode and a radial tensile stress in the non-reoxidized anode [112]. 2.4.7.", "Electrical Conductivity versus RedOx Cycles Robert et al. tested 800 μm thick anode-supports produced by slip casting with a porosity gradient created by sedimentation during the production process.", "The conductivity was measured on 120 mm diameter cells at 900 °C: it decreased from 2400 to 1300 S/cm after 7 RedOx cycles [90].", "A doubling in electrical conductivity was observed after a RedOx cycle at 850 °C of a Ni-YSZ composite based on coarse YSZ (from 500 to 1000 S/cm).", "After conductivity decrease due to nickel coarsening, the experiment was repeated on the same sample and the conductivity rose back to the highest level.", "Grahl-Madsen et al. reported that conductivity degrades faster after RedOx cycling [68].", "Ni-YSZ samples produced by tape-casting showed a conductivity decrease after the initial reduction [114].", "After the first RedOx cycle at 1000 °C, the conductivity increases to a value higher than the original value.", "After multiple RedOx cycles, the conductivity decreased and the degradation was faster than after the initial reduction.", "After removing Ni from the cermet with acid leaching, the ionic conductivity of the YSZ cermet was measured and showed a decrease due to cracks produced in the YSZ backbone by the RedOx cycle.", "A new proposed model included the increase in Ni contact after a RedOx cycle due to breaking of the zirconia skeleton.", "Further RedOx cycles will create too much porosity to maintain sufficient conductivity (see Figure 14).", "The conductivity of Ni-YSZ was measured at different temperatures and atmospheres (dry, wet or diluted hydrogen) [21].", "At 600 °C under wet hydrogen, the conductivity starts at 1200 S/cm and is constant over 150 h.", "RedOx cycles increase the conductivity to 2300 S/cm.", "At 850 °C under dry 40% H2 (diluted in He), the conductivity degraded by about 35% over 200 h.", "After a RedOx cycle, initial conductivity was restored at first.", "After the RedOx cycle, the conductivity degradation with time is lower over the same time period.", "An interesting point is that the dilution of dry hydrogen has an influence on conductivity losses, with a faster degradation in the case of He-dilution compared to Ar-dilution.", "A comparison of electrical conductivity for Ni-8YSZ and Ni-40CGO composites (on electrolyte supports) under RedOx treatments was performed by Iwanschitz et al.", "The conductivity was measured during 8 RedOx cycles at 850 and 950 °C: at higher temperature, the degradation was fast after 4 RedOx cycles and the Ni-CGO sample was not conductive anymore.", "In the case of Ni-YSZ, an increase in conductivity was observed during the first cycles (see Figure 15).", "The conductivity is always higher for Ni-YSZ than for Ni-CGO composites.", "The degradation after RedOx cycling is related to microstructure coarsening [81].", "Figure 14 Model proposed by Klemensø et al. including the increase of Ni contact after a RedOx cycle due to breaking of the zirconia skeleton.", "Further RedOx cycles will create too much porosity to maintain sufficient conductivity [114].", "Figure 15 Comparison between Ni-YSZ and Ni-CGO composite electrical conductivity under RedOx treatments [81].", "Liu et al. studied the conductivity of a NiO-YSZ anode of 800 μm thickness covered with a 10 μm thin YSZ electrolyte by electrochemical impedance spectroscopy (EIS) during reoxidation and re-reduction.", "EIS spectra were taken between 9 and 1000 kHz each minute during oxidation in air at 500, 600, 700 and 800 °C.", "The high frequency impedance spectra give the ohmic resistivity of the cell.", "The evolution in ohmic resistance during oxidation occurs in three phases: (1) low constant resistance; (2) a strong increase to a maximum value and (3) finally a decrease to reach an intermediate plateau.", "These stages correspond to the oxidation of the Ni particles until cutting the Ni conduction path followed by the creation of a new conduction path through NiO after volume increase (spongy-like porous NiO after reoxidation).", "The maximum ohmic resistance was reached after 3, 19 and 73 min at 800, 700 and 600 °C, respectively.", "No change was observed at 500 °C over 450 min due to slower kinetics.", "During reduction, the conductivity increases faster, meaning that the Ni network forms much faster [115]. 2.4.8.", "Temperature Variation during Oxidation Pomfret et al. observed a 20 K increase of temperature during anode-support reoxidation (at around 725 °C under air) using near infra-red imaging [116].", "With basic thermodynamic data, a temperature increase of 1678 K is calculated from the adiabatic reaction of an anode-support (final composition of 55 wt % NiO and 45 wt % YSZ) from Equation (7) [85]: (7) where nNiO and nZrO2 are the number of moles of NiO and zirconia, respectively, Cp,m is the molar heat capacity (at a constant pressure), ∆Hox,Ni is the enthalpy of nickel oxidation, ∆Hfusion,NiO is the fusion enthalpy of nickel oxide (the melting point of NiO is Tfusion = 1990 K), ∆Hα→β is the enthalpy for zirconia phase change (from α to β phase) and Tadiab is the calculated final temperature for the adiabatic reaction (Tadiab = 2478 °C).", "Cp,m is calculated from equation: Cp,m = a + bT; the heat capacities for pure α and β-zirconia and solid and liquid NiO were used for the calculation [29].", "Thermodynamic constants are given in Table 4.", "For the local anode temperature, the heat exchange with other parts and gases surrounding the anode should also be taken into account.", "This thermal effect can influence in situ expansion measurements (and even the furnace temperature, see Figure 16 in [117]), but it is nearly never taken into account in the different studies.", "After cracking the thin electrolyte, the combustion of the fuel at these locations creates hot spots with high water vapor that can induce accelerated nickel coarsening or cathode decomposition [85].", "Figure 16 Dilatometry measurements of oxidation for a YSZ composite bar infiltrated with 16 wt % Ni [117]. membranes-02-00585-t004_Table 4 Table 4 Thermodynamic constants for NiO and ZrO2.", "Cp,m is the molar heat capacity (at constant pressure), ∆Hox is the enthalpy of nickel oxidation (Ni +1/2O2 → NiO at 800 °C), ∆Hfusion the fusion enthalpy of nickel oxide (melting point of NiO is Tf = 1990 °C) and ∆Hα→β the enthalpy for zirconia phase change (from α to β phase).", "Cp,m is calculated from equation Cp,m = a + bT [29]. a (J mol−1 K−1) b (J mol−1 K−2) ∆ Hox,Ni (kJ mol−1) ∆ Hfusion (kJ mol−1) ∆Hα→β (kJ mol−1) NiO solid 46.81 8.46 × 10−3 239.8 [29] 50.66 [34] – NiO liquid 59.87 – – – – α-ZrO2 57.80 16.67 × 10−3 – – 4.75 [34] β-ZrO2 78.63 – – – – 2.4.9.", "Reoxidation by Ionic Current The ionic current coming from the cathode side can oxidize the Ni if no fuel is available at the anode side, as in the following equation: (8) The charge (in C) is directly calculated by the multiplication of the current density (A/cm2) by the active surface (cm2) and the time (s).", "Hatae et al. observed spongy-like structures of the Ni-NiO phase closer to the anode/electrolyte interface for a sample oxidized under N2 at 800 °C (YSZ electrolyte and 8YSZ-NiO active anode and support).", "The current conditions were 7.5 mA/cm2 for 30 min, giving 54 C.", "X-ray stress measurements in the electrolyte showed a lower compressive stress under the cathode (−298 MPa) compared to the side of the cell (−324 MPa) and to a non-reoxidized cell tested in similar conditions (−339 MPa) [118].", "Other studies from Hatae et al. reported contradictory results: one showed an activation of the electrochemical performance after oxidizing the anode with 15 C at 800 °C under nitrogen at current densities of 25 and 259 mA/cm2 [119]; another study presented degradation of the cell after a charge transfer of 15 C at a current density of 12.5 mA/cm2 [120].", "In both cases, the open circuit voltage (OCV) was constant.", "In a recent study on anode-supported cells, Hatae et al. showed an increase of electrochemical performance of about 36% after reoxidation via ionic current (250 mA cm−2 and 15 C = oxidation of 0.6% of Ni anode and anode support).", "In the same time OCV increased by about 2%.", "After 17 such RedOx cycles, the performance slightly decreased due to delamination between the anode and the electrolyte and cracks in the YSZ anode network.", "Two longer oxidation periods at the same current density (equal to 31% oxidation of the Ni) showed a decrease in OCV (−2%) but with an increase in performance at 0.25 A cm−2 of +26% [121].", "Sarantaridis et al. compared the oxidation in air with the oxidation by ionic current at 800 °C [112].", "Due to the non-uniformity of the electrochemical oxidation, the critical degree of such oxidation occurs at 3%, compared to 49%–75% by oxidation in air.", "Increase of the ohmic and polarization resistances was observed after electrochemical oxidation of nickel from a cell from the Forschungszentrum Jülich [122].", "As the peak frequency in the electrochemical impedance response and the OCV remained constant, the authors proposed a delamination-degradation mechanism occurring at the interface between anode support and active layer.", "Takagi et al. studied the influence of humidity in nitrogen during oxidation by ionic current.", "They analyzed the microstructure of a Ni-YSZ anode on a 500 μm electrolyte (YSZ) by 3D reconstruction with dual beam SEM-FIB and measured the electrochemical performance after 2 electrochemical RedOx cycles under dry N2 and 20% humidified N2.", "The humidity during oxidation makes the particles more spherical, which lowers their connectivity and decreases the electrochemical performance.", "The oxidation under dry conditions makes the particle size increase without change in the shape.", "Degradation is thus much lower in case of dry reoxidation by ionic current [123]. 2.4.10.", "Micro and Nano-Structural Changes upon Redox Cycling Macrostructural changes and physical property variations gave already some understanding on RedOx cycle effects on Ni-YSZ composite microstructures.", "The most used technique to observe post-microstructures is scanning electron microscopy (SEM).", "First observations showed coarsening of the NiO particles and microcracks in the YSZ skeleton [66].", "Zhang et al. observed a sponge-like aggregate of NiO crystallites.", "The re-reduction of this microstructure led to coarse Ni particles, suggesting a re-dispersion inducing some transport of nickel and nickel oxide during RedOx cycling [76].", "In parallel, Waldbillig et al. observed smaller pores in this sponge-like reoxidized NiO microstructure.", "In the same study, ex situ oxidation of a transmission electron microscope (TEM) lamella at 700 °C during 15 min showed nanometric polycrystalline NiO, even if the original nickel grain was a porous micrometric crystal [124].", "An in situ environmental SEM study showed live re-oxidation of nickel-YSZ composite under low pressure of 5–10 mbar of air.", "Isothermal oxidation at 850 °C showed a rapid oxidation with a separation of original nickel grains in 2–4 smaller particles that grew in the voids and out of the polished plane.", "In case of a temperature ramp oxidation, the oxidation starts at around 300 °C and progresses slowly until 450–500 °C, at which point the rate increases.", "This procedure presents the formation of a protective nickel oxide surface layer around the original nickel particle.", "The microstructure will depend on the oxidation condition of the composite; even the partial pressure of oxygen, which is much lower in the case of in situ SEM observation, can change the microstructure evolution [17].", "To understand the increase of the closed porosity by a factor of 3 before and after a RedOx cycle at 800 °C of a NiO-YSZ composite, Sarantaridis et al. used dual beam SEM-focused ion beam (FIB) to study the microstructure evolution of pure nickel particles of 5μm in diameter after oxidation at 800 °C.", "The surface of the sample using secondary electrons from the electron beam after oxidation is more textured and shows the sponge-like structure (see Figure 17 left).", "This effect is less pronounced when using the secondary electrons from the ion beam.", "To study the internal porosity, FIB was used to cut the particles after various oxidation times at 800 °C (see Figure 17 right).", "The evolution shows an increase of subsurface porosity during oxidation due to the outward diffusion of Ni2+ [50].", "Similar observations were done on Ni-YSZ composite reoxidized at 550, 800 and 1000 °C under air.", "Cross sections of the sample with SEM/FIB showed bigger NiO closed porosity at elevated temperature and small well dispersed NiO porosity at low temperature (see Figure 18) [85].", "This change in NiO closed porosity can be related to the outward Ni diffusion process during oxidation.", "At relatively low temperature (i.e., 550 °C), the Ni transport occurs via grain boundary of the NiO outer layer, and at elevated temperature (i.e., 1000 °C) the Ni transport occurs through the NiO crystal lattice [47].", "TEM observations showed porous NiO after an in-situ RedOx cycle.", "After the RedOx cycle, NiO grains grow out of the TEM-lamella plane and inside preexisting pores [125].", "Cross-section observation of the tested TEM lamella shows closed porosity inside the NiO (Figure 19).", "These observations can explain an irreversible strain after a RedOx cycle due to the re-oxidation process that increases the nickel oxide closed porosity.", "Understanding better the nickel oxidation process shows that the nickel coarsening during anode utilization is not the only cause of Ni-YSZ anode instability.", "Multiple RedOx cycles at elevated temperatures destroy the Ni-YSZ microstructure of an electrolyte-supported cell.", "A strong increase in porosity and in Ni particle size was observed after the process in Figure 20 [126].", "After an initial RedOx cycle, temperature programmed reduction (TPR) showed a lower temperature of reduction and a faster reduction rate [76].", "X-ray diffraction (XRD) revealed a broadening of the NiO peaks [127,128].", "These two observations confirm the decrease of particles and crystallites size during the Ni reoxidation process in a Ni-YSZ composite.", "Figure 17 Left: SEM of (a) as received Ni and (b) fully oxidized Ni (NiO) particles.", "The secondary electron images were recorded using a beam energy of 20 keV.", "Right: FIB cross-sectional secondary electron images of Ni particles oxidized at 800 °C for (a) 30 s; (b) 60 s; (c) 90 s; (d) 180 s; and (e) 300 s.", "Image (f) is the same particle as in (e) but obtained using the secondary ion signal [50].", "Figure 18 Secondary electron image from FIB cross-section from half-cells after one RedOx cycle (a) at 550 °C (lower magnification); (b) at 550 °C (higher magnification); (c) at 800 °C and (d) at 1000 °C.", "NiO contains small pores after a RedOx cycle at 550 and 800 °C but a single big pore after a RedOx cycle at 1000 °C.", "Dark grey is YSZ and light grey is NiO.", "The vertical lines come from the FIB milling process (“curtain effect”) [85].", "Figure 19 Cross-section of a transmission electron microscope (TEM) lamella after an in situ RedOx cycle, showing the hilly surface and closed porosity of the nickel oxide after reoxidation [129].", "Figure 20 Fine Ni-8YSZ anode before (left) and after (right) eight RedOx cycles at 950 °C (SEM, backscattered electron detector, 10 kV) [126]. 3-D reconstructions using FIB-SEM microscopy of oxidized Ni-CGO cermet at 510 and 575 °C showed nucleation of temperature-dependent pseudo-Kirkendall voids.", "Larger pores were observed at the highest oxidation temperature [65].", "Microstructural evolution of Ni-YSZ composite was observed by X-ray computed tomography.", "Limited microstructural change was seen after 10 min oxidation steps at 500 °C but a porous NiO layer of about 700 nm was reported after 10 min at 700 °C [130]. 2.4.11.", "Electrochemical Performance and Electrochemical Impedance Spectroscopy The electrochemical performance after a RedOx cycle can vary a lot.", "In case of ASC, a decrease in OCV can occur, indicating the thin electrolyte to crack [10,90,113].", "The performance can increase due to, first, a better electrical contact between cell and current collecting layer [131] and, second, an activation [73,132] or re-activation after degradation [133] of the active anode.", "Pihlatie et al. observed a decrease in Rp after a RedOx cycle at 650 °C and a small decrease in Rs after a RedOx cycle at 850 °C, of symmetrical Ni-ScSZ anodes on a ScSZ electrolyte-supported cell.", "Microstructural observation revealed a finer microstructure after the 650 °C RedOx cycle and cracks in the electrolyte after the 850 °C RedOx cycle [73].", "In many cases, the performances decrease due to an increase in polarization resistance (Rp) [16,66,81,126,127,131] and in some cases an increase in ohmic resistance (especially for Ni-CGO, see Figure 21) [81,126].", "Iwanschitz et al. showed the evolution of the imaginary part of impedance versus frequencies after RedOx cycles for Ni-8YSZ and Ni-40CGO [81,126] (see Figure 21).", "After a cycle at 950 °C, the Ni-CGO anode showed an increase of the peak at 1 Hz (corresponding to the conversion and diffusion impedances [134,135]) as well as of the ohmic resistance Rs.", "This increase in peak height means a change in the gas transport process, while the Rs evolution is linked to the electronic conductivity decrease in the Ni-40CGO layer (see Figure 15).", "The Ni-YSZ anode showed an increase of the high frequency peak (corresponding to the charge transfer impedance [136,137]) from 1 kHz to 10 kHz.", "The variation in frequency after the RedOx cycles means that the capacity layer between Ni and YSZ is changed.", "The change in peak height showed a degradation of the anode due to a decrease in active sites.", "A correlation study between the electrochemical characteristics and the microstructural evolution was done using 3D microstructure reconstruction with a FIB/SEM microscope.", "RedOx cycles of a Ni-YSZ thin anode on an electrolyte-supported cell at 1000 °C showed electrochemical performance degradation: Anode polarization losses increased from about 0.06 initially to about 0.09 Ω cm2 after the fourth RedOx cycle.", "This was correlated to a decrease in triple phase boundary (TPB) length of the anode from initial 2.49 to 2.11 μm−2 after 4 RedOx cycles [138,139].", "Figure 21 Impedance spectra at OCV during RedOx cycling at 950 °C of (a) Ni-40CGO (Ce0.6Gd0.4O2−d) and (b) Ni-8YSZ anodes with a 8YSZ electrolyte support.", "Top: Nyquist plot; bottom: complex impedance plot [81,126].", "Laurencin et al. studied Kerafol 3YSZ supports with a 8YSZ porous interlayer (15 μm) and a NiO-8YSZ anode of 25 μm (with 31% porosity in oxidized state) [127].", "RedOx cycles were performed during 30 min under air at 800 °C.", "The impedance spectra were fitted with an equivalent circuit based on a resistance (Rs, ohmic resistance) in series with three RC processes of a resistance and a constant phase element in parallel.", "This gives three semi-circles of low (0.4–0.8 Hz), intermediate (6.2–10.9 Hz) and high (330–590 Hz) frequency phenomena.", "Ohmic resistance is constant while the polarization resistances at high and low frequency increase with RedOx cycling.", "The high frequency response is related to charge transfer and the low frequency response to gas diffusion and conversion.", "The authors explained the peak increase by the densification and the deterioration of the anode microstructure.", "Müller presented the evolution of the imaginary part of impedance versus frequencies after RedOx cycles at 950 °C [16] (Figure 26).", "In general, he observed an increase in the peak around 1 kHz and in some cases a slight increase in the low frequency peak around 1 Hz.", "All studies on ESC Ni-YSZ revealed an increase of the complex impedance around 1 kHz during RedOx cycling.", "This is linked to the charge transfer at the Ni-YSZ anode active sites; an increase in complex impedance means a deterioration of the microstructure at the anode/electrolyte interface. 2.4.12.", "Single Chamber SOFC In the case of a single chamber SOFC, the problem is different as both reducing and oxidizing gases are introduced together in the fuel cell.", "The specific activities of the two electrodes will produce a potential difference and generate current.", "Jaques-Bedard et al. observed an oscillation of the potential of a Ni-YSZ anode supported cell under a methane-to-oxygen ratio (M/O) lower than 2.", "This oscillation with a period of 20 s is related to the reduction and oxidation ongoing at the nickel surface.", "The degradation is more elevated for M/O < 2 and is explained by higher Ni evaporation at the fuel entrance and damages due to RedOx cycles [140].", "Similar tests were done adding anode resistivity measurements.", "A voltage decrease was correlated to the anode resistivity increase; it was concluded that reduction-oxidation of Ni in the anode induced the voltage oscillation [141].", "To clarify the effect of flowing both reducing and oxidizing gases over the anode, Kellogg et al. studied the Ni-YSZ anode in a double chamber, electrolyte-supported cell configuration.", "They flew 2/3 H2 and 1/3 O2 diluted in 95% of Ar over the anode, and pure oxidizer gas over the cathode.", "Oscillations of the open circuit voltage were observed around the equilibrium voltage of NiO/Ni at 600 °C.", "The explanation is an oxidation of the nickel and a re-reduction due to accumulation of H2 (the period is about 70 s in this case).", "Electrical conductivity measurements under these conditions showed a similar oscillation.", "When the H2/O2 mixture was flown over the cathode (with reducing gas over the anode) no variation was observed [142]. 2.5.", "Summary of the RedOx Instability One of the main limitations of nickel-based SOFC anodes is its RedOx cycling instability.", "The RedOx instability is coming from the volume change of nickel between its reduced and oxidized states.", "The volume increase during nickel oxidation induces an expansion of the composite.", "This expansion has three origins: (1) The reorganization of the metallic nickel during utilization; (2) the fast oxidation kinetics of the nickel at the operating temperature (between 600 and 800 °C) and (3) the closed porosity formation during the oxidation process.", "At low temperature or high oxygen partial pressure, the oxidation-limiting factor is the solid-state diffusion (which is thermally activated) giving a homogeneous oxidation of the full anode layer.", "In opposition, at elevated temperature and low oxygen partial pressure, the oxidation-limiting factor is the O2 gas diffusion through the oxidized anode layer leading to an inhomogeneous oxidation and higher layer internal stresses.", "Increasing reoxidation temperature will increase the expansion of the anode and the damages to the ceramic network.", "The anode-supported cell (ASC) configuration is the most sensitive cell design: an anode expansion of 0.2% already induces cracks in the thin electrolyte.", "For the electrolyte-supported cells (ESC), the expansion limit before delamination of the anode is increased to 0.5%.", "In the case of cells on inert supports (RedOx stable metal or ceramic support), the expansion limit is even higher (around 1%).", "Various causes might induce anode oxidation during operation: air leakage (lack of fuel, shutdown and start-up without reducing gas, compressive sealing), high current demand, and fuel starvation.", "In the last two cases, the anode will oxidize due to ionic current (O2−) coming via the electrolyte.", "With these kinds of RedOx cycles, only a low amount of oxidized nickel (small degree of oxidation) will cause damages to the cell.", "After a RedOx cycle, the electrochemical performance of a cell might either decrease or increase depending on the severity of the cycle.", "The ohmic resistance can decrease after a RedOx cycle as shown by the electrical conductivity increase, but the degradation is often accelerated due to ceramic network damages.", "Concerning the polarization resistance (Rp), if the RedOx conditions are severe (high temperature), as is normally the case for ECS, the ceramic network suffers and a decrease in performance is measured due to a decrease in triple phase boundary (TPB) length.", "On the opposite, if the RedOx cycle conditions are soft (RedOx cycle at low temperature, 650 °C), changes in the nickel morphology may induce even an increase in the TPB length and hence a lowering of Rp.", "In case of an ASC, if the thin electrolyte cracks severely, the cell is destroyed.", "If the cracks are not too severe, the open circuit voltage will drop but the local temperature increase can nevertheless lead to enhanced performances under low fuel utilization.", "In general, published results do show a relatively large scatter which can be attributed to the variation of (1) the microstructure, including particles size and porosity (parameters not always given in the literature); (2) the composition of the sample; (3) the testing procedure and setup (duration and oxygen partial pressure) and (4) the design of the cell (including the active functional layer, the interlayer and the contact layer of the anode).", "Directions to improve the RedOx stability of the anode can be suggested from the results reported in this chapter.", "The next chapter will present and organize published solutions.", "They are separated in two families: (1) Solutions coming from the system itself and (2) solutions based on variations of the cell and its materials.", "Unfortunately not all solutions are precisely presented in the literature, especially those based on a patent.", "On the opposite, some alternatives, such as on ceramic anodes, are so largely described that they could be a subject for a review on their own. 3.", "RedOx Solutions This chapter attempts to give a complete overview of the RedOx solutions reported until now in the scientific community and in patents.", "A review has been made by Wood et al. from Versa Power Systems Ltd.", "(VPS) for small-scale residential and industrial power generation (3–10 kWe) based on anode-supported cells [143,144].", "The potential solutions can be divided in two general families as summarized in Figure 22: System solutions aim at keeping an oxygen partial pressure low enough to protect the anode from oxidation based on the global balance of plant of the SOFC system.", "They have two challenges: (1) compensate the RedOx limitation of anode materials; (2) include safety implementation of the anode and fuel processing gas.", "Hydrogen mixtures can explode below the autoignition temperature and carbon monoxide can be dangerous because of its flammability, toxicity and its propensity to react with nickel at a temperature below 230 °C to form the volatile and toxic nickel carbonyl.", "System solutions must protect the whole stack under normal events including varying power output, start-up and shutdown.", "But the unusual events are more dangerous for the stack, such as (1) system shutdown without fuel but with power available, and (2) emergency stop of the system (“blind shutdown”), without fuel and power.", "System solutions are grouped into dependent (to the system design), passive (no electrical power needed) and active (requiring the use of electrical power) measures.", "For small stacks (<1 kWe), system solutions are too expensive and good alternative ways must be found in the second approach.", "Materials, cell and stack design solutions, such as alternative anode materials or optimization of the anode composition and microstructure.", "This approach is clearly passive and its cost is likely to be minimal.", "Therefore, while giving a brief overview of system solutions, this review will focus more on materials and design solutions.", "A summary of the RedOx cycle degradation measurement as a function of the different solutions, especially from the second group, is presented in Table A1 (Appendix). 3.1.", "System Solutions 3.1.1.", "Dependent System Solutions In the anode gas recirculation, the anode atmosphere will stay longer in a reducing environment upon fuel supply interruption; only about 10% to 15% of the anode gas mixture would be lost and would need to be changed (by a reducing or neutral gas).", "Figure 22 Summary of the solutions for anode RedOx instability [129].", "The fuel enclosure solution is similar to the “anode recirculation” solution but with a closed circuit, hence 100% of the gas is recirculated. 3.1.2.", "Passive System Solutions Metal hydrides trap hydrogen within an alloy.", "It is the best technology of a hydrogen container.", "When heat is applied, the gas is released.", "Reversible materials such as magnesium hydrides (MgH2) are typically used at 300 °C.", "At 650–700 °C no material is known to possess the same properties and more investigations are needed, but the high (endothermal) enthalpies of formation of these materials do not seem to be an issue for the SOFC protection.", "Mukerjee et al. describe some candidate materials [145].", "Reversible oxygen getter and sacrificial materials solutions use unstable materials, such as nickel itself, to chemically react with any free oxygen that enters into the anode vicinity at high temperature.", "It would keep the oxygen partial pressure in the anode side low or the potential of the anode in a region where there is no oxidation of anode active materials.", "This approach is presented by England et al. [146] and Haltiner et al. [147] from Delphi company.", "Assuming that liquid water is available, it can be added to the system and vaporized by the thermal energy contained in the hot balance of the SOFC plant.", "The reformer can be used to set up a slightly reducing gas by oxidizing some of the reforming catalyst as shown for nickel in Equation (1) (from right to left).", "As an alternative to the reformer, an additional nickel containing bed can be used.", "This steam purge can reduce the cell degradation by a factor higher than 30 [143,144].", "Valves can be closed by gravity when the partial pressure of oxygen increases to a threshold value.", "This can be coupled with the use of an oxygen getter [147].", "Using ceramic-glass sealing, the emergency valves closing can protect the stack during 15 h at 750 °C, which gives enough time for stack cooling [143,144].", "By having an alcohol-water mixture, the fuel composition is adjusted to give a desired purge gas.", "The idea is to use the thermal energy contained in a hot SOFC to drive the endothermic reforming of the fuel (ethanol) (Equation (9)) [148]. (9) Thermal cracking of a stored fuel source uses the same idea as before but uses the cracking reaction instead (Equation (10)). (10) The activated carbon solution approach uses a carbon bed, which is an irreversible solution because at high temperature, air oxidizes the carbon to produce carbon monoxide and carbon dioxide gas [145]. 3.1.3.", "Active System Solutions The use of a partial oxidation reformer can generate a suitable reducing gas for anode protection [149].", "As explained in Section 2.2.2, the cell voltage is directly related to the gas composition at the anode and cathode through the Nernst potential.", "Thus, if an external voltage is applied to a cell or stack, this cell reversal is expected to reverse the flow of oxygen ions to maintain the anode at a safe oxygen partial pressure and protect the oxidation of the metal.", "The theory predicts this protection voltage on a simple gas/metal oxide/metal system but the cermet mixture makes it different [47].", "This concept is outlined by Mukerjee et al. from Delphi company [145].", "Recently, Young et al. studied the application of a constant cathodic current or potential to the anode during RedOx cycles.", "An ESC with a Pt counter, a Pt reference and a NiO-8YSZ (56–44 wt %) working electrode (0.4 cm2) was tested with constant potential or current of −150 mV, −350 mV, −6.5 mA and −17.5 mA under humidified hydrogen and air for 20 to 80 min at 800 °C.", "Main results are that under potentiostatic mode, the ASR decreased in opposition to galvanostatic mode where the ASR increased [150].", "Further investigations, in particular on the microstructure, should be done to understand these results.", "The independence of cells would allow changing the current density for each cell.", "It could also use the working cell in a similar manner as explained in the previous paragraph.", "But in case of a fuel supply problem, this approach is limited.", "This idea was presented by Backhaus-Ricoult et al., who showed an activation during 2 RedOx cycles at 720 °C without indication on the anode composition [151].", "As the kinetics are strongly dependent on temperature, fast cooling of the stack with a rate of 3 °C min−1 or higher (between 800 and 600 °C) will slow down sufficiently the kinetics so that standard Ni-YSZ anode support cells can withstand the oxidation [152].", "Treating the air with a purification device to separate the oxygen and the nitrogen, the nitrogen is flown to the anode compartment and oxygen enriched air at the cathode side.", "Purified air can protect the anode against reoxidation during cooling down [153]. 3.2.", "Stack Design 3.2.1.", "Planar Design The planar design is the most studied one because it can reach higher power volume density.", "The design of such a stack can be optimized to limit reoxidation of the anode supported cell.", "Van herle et al. calculated the partial pressure of oxygen depending on the fuel utilization (Fu) for an open post-combustion design with counter flow, the so-called R-design.", "The reoxidation of Ni was obtained already at Fu of only 64% [33].", "In a similar manner using computational fluid dynamics (CFD) modeling of the partial pressure of oxygen, Larrain et al. calculated the risk of oxidation versus the Fu.", "For a counter-flow configuration, the Fu limit is given as a function of temperature and hydrogen flow rate.", "At 710 °C under adiabatic conditions the maximum Fu is decreasing with increasing fuel flow rate from 92% at 200 mL/min to 89% at 400 mL/min.", "For the co-flow case, the limitation is only determined by the total fuel utilization [11].", "Implementing the leakage in a compressive seal in the CFD model, Wuillemin et al. showed that high Fu would decrease the active cell area.", "Using mica as sealing in an R-design configuration, the reoxidation of the active zone starts at 30% Fu; at 68% Fu the decrease in active zone is about 1.7% [154].", "Based on CFD modeling, the flow design of the planar cell was optimized to limit the reoxidation of the cell [155]. 3.2.2.", "Tubular Design This design can be seal-less and is known to resist transients [20].", "The University of Birmingham studied the behavior of tubular anode supported cells with 200 μm anode thickness, 15 μm electrolyte thickness and with 2 mm of external diameter (produced by co-extrusion by Adaptative Materials Incorporated, USA) [20,156].", "The electrochemical degradation and linear expansion were studied against temperature (at 600, 700 and 800 °C) and oxidation time of RedOx cycles (5 min and full RedOx cycle).", "The degradation increases with increased temperatures after a full RedOx cycle.", "The cell no longer worked despite relatively small expansion (see Table 5).", "Other studies also showed high degradation of cell performances under RedOx cycles [104].", "Anode-supports with 10 mm of diameter showed high degradation as well (strength, conductivity, electrochemical) after 8 h RedOx cycles at 800 °C [157].", "As the tubular cell can withstand relatively high cooling rates, an optimal cooling rate should be found to limit the degradation of the RedOx cycle by slowing the kinetics without increasing the degradation due to thermal shock [158].", "In all these studies, the electrolyte is deposited exterior of the anode support.", "A small expansion of the support will then create large tensile stresses in this layer.", "If the electrolyte was deposited inside the support, then it could even be under compressive stress if the anode expands.", "This might be a solution for the tubular design.", "The mixed design aims to combine advantages of the seal-less tubular design with the high volume density of the planar design [159]. membranes-02-00585-t005_Table 5 Table 5 Influence of temperature and time of reoxidation on the electrochemical performance and the linear expansion of tubular anode supported cells [20].", "T/°C 52 RedOx cycles of 5 min, ∆i/i at 0.5 V After first full oxidation cycle, ∆i/i at 0.5 V Expansion during first full oxidation Time to full oxidation (h) 600 −0.38%/cycle −35% 0.20% 4.5 700 −0.42%/cycle −61% 0.33% 3.0 800 −0.44%/cycle −72% 0.46% 0.5 3.3.", "Cell Design 3.3.1.", "Cathode Supported Cell (CSC) The cathode supported cell was used in Siemens-Westinghouse technology and showed very long operating times (>40,000 h) with low degradation, but no mention on RedOx cycling was given [1].", "The main drawback of the Siemens-Westinghouse technology is the elevated price of cell production.", "Huang et al. presented an electrochemical activation after 2 RedOx cycles for a 1 mm LSM porous support with a YSZ electrolyte and a noble metal anode based on Pd (1 μm median size) and YSZ (0.17 μm median size).", "At 800 °C, the power density was 0.15 Wcm−2 at 0.5 V [160].", "No mechanical model describes this configuration under a RedOx cycle. 3.3.2.", "Electrolyte Supported Cell (ESC) The electrolyte supported cell is a robust cell under RedOx conditions [106], but due to the high ohmic loss in the thick electrolyte at low temperature (700–800 °C), higher temperature must be used that makes the impact of the faster reoxidation important even for this cell configuration.", "ESCs under RedOx treatments have been well studied especially by Hexis and Kerafol [161,162].", "In 2004, Hexis proposed to add doping elements to the nickel oxide to increase RedOx stability.", "They then showed 40% performance degradation over 3 RedOx cycles [161].", "Four years later, the degradation of a 5-cell stack (with 120 mm diameter cells) over 11 RedOx cycles was lowered to 24% of area specific resistance (ASR) increase.", "Button cells showed about 40% degradation over 50 RedOx cycles (the first 30 RedOx cycles presented only small degradation) [163].", "By changing the electrolyte composition from 8YSZ to 10ScSZ, a decrease of 50 °C in operating temperature could be brought about maintaining similar performance [164].", "This also enhances the RedOx stability of the cells: a 5 cell-stack did not show any degradation over 12 RedOx cycles at 900 °C but then lost about 160 mV under constant current density for the last 8 RedOx cycles.", "A full system worked for 15,000 h with 4 thermo-RedOx cycles and 3 RedOx cycles with 1.9%/kh degradation.", "Further optimization work on the anode composition showed that the Ni-8YSZ is better at 950 °C under RedOx conditions compared to Ni-40CGO, due to better electrical conductivity.", "At 850 °C the effect is reversed and the Ni-40CGO is more stable due to a constant polarization resistance [81].", "The Ni-40CGO thin anode was studied with in situ X-ray diffraction, the time for full oxidation of the nickel in the anode is 4 min at 650 °C and only 0.5 s at 850 °C [64].", "Development on the anode microstructure and composition showed that coarse NiO-YSZ maintains a high conductivity under RedOx cycling and 40:60 vol % Ni:YSZ composition is more stable than 35:65 vol % [126] .", "In parallel, Kerafol observed a constant ASR for 3 RedOx cycles at 850 °C using a 10Sc1CeSZ electrolyte and a Ni-8YSZ anode.", "During 3 further RedOx cycles, the ohmic and anodic polarization resistances increased [162].", "The total ASR increased from 0.37 to 0.47 Ohm cm2 after 6 RedOx cycles.", "The microstructural analysis showed that the porosity of the tested cell had increased strongly.", "They observed a large scattering of the measurements because the RedOx cycles influenced also the contacting of the anode [131].", "Microstructure optimization showed that coarse NiO (keeping the same YSZ) enhances the RedOx stability: After 10 RedOx cycles of more than 3 h at 850 °C, cell performances stayed stable at 0.7 A cm−2 at 0.7 V [165].", "More recently, Staxera GmbH reported a study on 30 cell-stacks of 3YSZ thick electrolyte, Ni-CGO anode and LSM-YSZ cathode (128 cm2 active surface).", "After 80 thermo-RedOx cycles (cooling down without protective gas from 850 °C at a rate of 100 °C/h), the power output decreased by about 10% (0.125% power degradation per cycle).", "By changing the reduction conditions from 30 min at 700 °C to 5 min at 800 °C, the degradation per cycle increased to 0.44%.", "Pure RedOx cycles (20 min air flushing at the anode at 800 °C) degraded the stack power output of 1% per cycle [166].", "Ouweltjes et al. tested a 25 cm2 electrolyte supported cell (ECS) of 3YSZ with an AFL of 80 wt % of 10CGO and 20 wt % of infiltrated NiO.", "The anode-contacting layer was based on La0.9Mn0.8Ni0.2O3 30 wt % and 70 wt % Ni.", "This cell was RedOx-cycled for 120 min in air at 850 °C.", "A degradation of 10% was measured after 50 cycles and 24% after 100 cycles.", "Performances started at 0.36 A/cm2 at 0.7 V and ended at 0.28 A/cm2 at 850 °C, with 50% H2–50% H2O as fuel mixture [167].", "Ukai et al. proposed to enhance the strength of the electrolyte by adding 0.5%–5% of Al2O3 to 3–6 mol % ScSZ to obtain RedOx stable cells.", "They claimed to achieve constant OCV and performance after RedOx cycles at 950 °C [168].", "Weber compared ESCs with ASCs configuration over 50 short and 50 long RedOx cycles (applied successively); during the long RedOx cycle, the OCV dropped to zero for all ASCs and the performance degraded rapidly for all ESCs [169]. 3.3.3.", "Metal Supported Cell (MSC) This cell configuration should be the most stable under RedOx conditions as shown in Section 2.4.6 [106].", "The configuration can be made as (1) Substrate/Anode/Electrolyte/Cathode (S/A/E/C) [170] or reversed with (2) S/C/E/A [171].", "Usually, due to cost limitations, an iron-based support is chosen.", "The benefits with configuration (1) are more freedom on the cathode composition.", "The major limitation is interdiffusion of Fe (from the metallic support) and active Ni (from the anode).", "A solution for a stable active anode is to impregnate the support with ceria or other salts after the electrolyte densification [170].", "The benefits of configuration (2) are (a) no interdiffusion of Ni/Fe; (b) less corrosive cathode atmosphere for the metal support and (c) more freedom in the anode composition.", "One limitation is however chromium poisoning of the cathode; the composition should be tuned to limit this degradation.", "The German Aerospace Center (DLR) SOFC technology is based on plasma sprayed layers on a metal substrate.", "In 2004, they showed a CroFer22APU porous structure with a Ni-YSZ anode under 7 RedOx cycles (40 min of oxidation at 800 °C) with an electrical conductivity decrease from 2200 to 2000 S/cm during the first 3 RedOx cycles, which then stays constant.", "During these cycles, both OCV and performance remained constant (1.03 V, and 400 mW/cm2 at 0.7 V 800 °C) [172].", "Three years later, 10 RedOx cycles could be performed with only small OCV decrease from 1.049 to 1.037 V (0.11% degradation per cycle).", "The performance stayed stable around 149 mW/cm2 at 800 °C and about 0.75 V [173].", "After optimization of the layers, more than 20 full RedOx cycles were performed on 12.5 cm2 cells without measurable degradation in OCV and less than 2.5% degradation in power density [174].", "A stack of two cells with 82 cm2 active surface each, tested over 20 RedOx cycles at 800 °C during 1 h under pure oxygen, showed an increase in cell performance during the first five RedOx cycles after long period of 1250 h testing (for cell-1 from 128 to 156 mW/cm2 and cell-2 from 158 to 177 mW/cm2).", "After the 20 RedOx cycles, the performance of cell-1 and cell-2 degraded about 12.5% and 5.6%, respectively.", "This was attributed to increases in anode polarization resistance (+180%) and in electrolyte ohmic resistance (+50%) [133].", "Metal supported cells produced by tape-casting with an anode of CrFe (350) or CrFe and YSZ were presented by Blennow et al. [175,176].", "Sintering was done under reducing atmosphere with ScYSZ electrolyte, followed by infiltration with 20CGO with 10 wt % NiO and calcination for 2 h at 350 °C.", "The RedOx stability of these cells was compared to anode supported cells based on Ni-YSZ (with support thickness of 1, 0.4 and 0.5 mm for ASC1 (from FZJ), ASC2 and ASC3, respectively [14]) under 50 RedOx cycles of 1 min at 800 °C and 50 RedOx cycles of 10 min at 800 °C (see Figure 23).", "During the first 50 cycles, OCV was constant and performance slightly increased.", "During the next 50 cycles, OCV and performance decreased about 15% to 20%.", "A big difference could be observed between metal and Ni-YSZ anode supported cells.", "A tubular metal supported cell (based on the configuration: Metal support/porous YSZ/dense YSZ/porous YSZ/metal support) was infiltrated by LSM (twice) and Ni (10 times).", "After each infiltration, the cell had to be fired at 650 °C.", "After 5 RedOx cycles, 26% degradation was observed with an initial power density of 650 mW/cm2 at 0.7 V at 700 °C under H2 and pure O2.", "For long-term stability, the Ni needs to be pre-coarsened at 800 °C, giving performance of 80 mW/cm2 at 700 °C [177].", "These results of RedOx stability of metal supported cells make them a very interesting technology for the future.", "Long-term stability of more than 10,000 h still remains to be confirmed.", "Figure 23 RedOx stability of anode supported cells (ASCs) (with support thickness of 1, 0.4 and 0.5 mm for ASC-1 (from Forschungszentrum Jülich), ASC-2 and ASC-2, respectively [14]) compared to metal supported cell (MSC), under 50 RedOx cycles of 1 min and 50 RedOx cycles of 10 min at 800 °C.", "Top: open circuit voltage, bottom: normalized performance at 0.7 V [175]. 3.3.4.", "Inert Substrate Supported Cells (ISSC) An inert non-conductive substrate of Ni-doped MgO-YSZ composite was used by Tokyo Gas for segmented-in-series (SIS) cells with Ni-YSZ anode.", "Two RedOx cycle procedures were used: (1) start-up and cool-down under air/water vapor (a/w) ratio of 0.5 and (2) 1.5 for 30 min at 775 °C under similar a/w.", "The open-circuit voltage stayed constant and the electrochemical performances decreased a few percent after 20 RedOx cycles of type 1 and isothermal cycles (type 2) [178].", "Another study showed a SIS cell based on a flattened partially stabilized zirconia tube with a 70:30 wt % NiO:YSZ anode, 8YSZ thin electrolyte and LSM-YSZ cathode.", "The RedOx cycles of 30 to 40 min under air at 800 °C were applied 19 times without noticeable electrochemical performance loss (see Figure 24, note that the OCV is not shown) [179].", "Sr0.8La0.2TiO3 porous support coated with NiO-Ce0.8Sm0.2O2 (SDC), NiO-YSZ and YSZ thin electrolyte presented impressive performance (0.9 A/cm2 at 0.5 V) and RedOx stability at 800 °C (see Figure 25) [180].", "Figure 24 Voltage with time during RedOx cycles 800 °C of segmented-in-series (SIS) cells on a flattened partially stabilized zirconia tube support (under fuel, i = 0.9 A/cm2).", "In the first part of the test shown in (a), 12 SIS cells on one side of the module were tested during 7 cycles.", "The module was cycled to room temperature and then back to 800 °C before the second part of the test (b), where 9 SIS cells on the other side of the module were tested during 12 cycles.", "Arrows 1 and 2 indicate when the module was left overnight at 800 °C in hydrogen without cycling.", "Arrow 3 indicates a longer-than-usual (1 h) fuel feed [179].", "Figure 25 Time dependence of cell voltage of a Sr0.8La0.2TiO3 supported-cell with Ni-Ce0.8Sm0.2O2, Ni-YSZ anode and YSZ thin electrolyte over 7 RedOx cycles at 800 °C (under fuel, i = 0.9 A/cm2).", "The cell is alternatively exposed to dry H2 for 45 min and air for 30 min [180]. 3.3.5.", "Anode Supported Cell (ASC) The anode supported cell technology is the most sensitive configuration to RedOx cycling but currently also the most popular one owing to high performance at low temperature thanks to the dense thin electrolyte.", "The next sections of this chapter will mostly describe the strategies used to enhance the RedOx stability of ASCs. 3.4.", "Modification of the Microstructure In order to enhance anode redox resistance, anode microstructure evolution needs to be investigated under RedOx cycles.", "This sub-section reports the state-of-the-art. 3.4.1.", "Anode Functional Layer, Anode Support and Anode Current Collecting Layer Based on a mechanical model, it was shown that the most important goal is to limit the anode support (AS) expansion and in a second step to limit the anode functional layer (AFL) expansion (see Section 2.4.6) [109].", "The composition of the two layers can be different: the microstructure of the anode support should be more porous to maximize the gas transport and should have a high electrical conductivity, whereas the AFL should be denser and finer to increase the electrochemical active sites (or triple phase boundaries).", "Waldbillig et al. separated the functions of the two layers and tested the structures for RedOx stability [41].", "This approach was also followed by other authors [14,181,182].", "In the electrolyte-supported case, Müller et al. separated the function of the AFL and the current collecting layer (CCL) and tested structures for RedOx stability [16,183].", "He presented the evolution of the imaginary part of impedance versus frequencies after RedOx cycles [16].", "He noted that the frequency peaks depend on the microstructure, the composition and the presence of a current collecting layer.", "Sample composition and electrochemical measurements after RedOx cycles at 950 °C are described in Table 6 and Figure 26.", "Figure 26 Electrochemical impedance spectroscopy at open circuit voltage (OCV), of electrolyte supported cell after RedOx treatments at 950 °C of sample composition (a) A; (b) B; (c) C and (d) D described in Table 6 [16].", "Without CCL, the imaginary part of impedance increases strongly around 1 kHz (Figure 26a).", "These frequencies correspond to the charge transfer process in the Ni-YSZ anode [136,137].", "The cell after testing presented a large surface of total anode delamination (Figure 11 left).", "Adding a CCL on the active anode (sample B, Figure 26b) increases the low frequency peak (related to gas conversion and gas diffusion [134,135]).", "After RedOx cycles, the degradation at charge transfer frequencies is imitated even if the cell showed delamination between AFL and CCL (Figure 11right).", "With a finer AFL and sintered CCL (sample C, Figure 26c), both low (1 Hz) and high (1 kHz) frequencies were decreased.", "Changing NiO by Ni(OH)2 seems to enhance strongly the RedOx stability of the AFL (Figure 26d).", "This could be due to a difference in porosity of the active layer. membranes-02-00585-t006_Table 6 Table 6 Composition and microstructure of the active and current collecting layer anode (the composition is always 65:35 mol % Ni:8YSZ for all layers and the active layer is sintered in all cases at 1350 °C) [16].", "Sample Active functional layer Current collecting layer A NiO (1 μm)-8YSZ (0.8 μm) None B NiO (1 μm)-8YSZ (0.8 μm) Ni-8YSZ (no sintering) C NiO (0.5 μm)-8YSZ (0.5 μm) NiO (0.5 μm)-8YSZ (0.5 μm), sintered at 1250 °C D Ni(OH)2 (0.5 μm)-8YSZ (0.5 μm) NiO (0.5 μm)-8YSZ (0.5 μm), sintered at 1250 °C 3.4.2.", "Particles Size As early as 1996, Itoh et al. recognized the importance of the anode base material particles size for the stability of the cell.", "They showed (but only during a reduction reaction) that the use of a YSZ bimodal distribution (fine and coarse) led to a more stable anode [184].", "More recently, Fouquet et al. measured the expansion of samples made of different NiO/YSZ particles size and sintered at 1300 °C.", "The expansions depended on the NiO/YSZ particle size ratio as follows: The lower expansion is for 0.5/0.2 followed by 0.5/0.8 and by 1.4/0.2, with particles size in μm.", "They found that the NiO particle size and the ratio between the particle size NiO/YSZ is the main factor for expansion during oxidation, but only three samples were tested [66].", "Robert et al. changed the proportion of fine to coarse YSZ particles.", "They observed that the expansion is bigger in case of high content of fine YSZ [185].", "Waldbillig et al. observed about 2.5% expansion for a fine microstructure and only 0.23% for a coarse microstructure during a RedOx cycle at 750 °C [41].", "Design of experiment (DoE) approach was used to optimize the anode-support properties like RedOx stability, electrical conductivity and “surface quality”.", "The varied parameters were coarse and fine NiO and 8YSZ particles (with dV50,coarse ≈ 9 μm and dV50,fine ≈ 0.5 μm), composition (from 40 to 60 wt % NiO) and pore-former addition (from 0 to 30 wt %).", "Statistical analysis over 46 samples of 25 different compositions showed that the presence of coarse YSZ reduces RedOx expansion whereas changing the NiO particle size did not have a significant effect [86].", "From the DoE study, three different anode-supported compositions (with 40, 50 and 60 wt % NiO) were tape-casted and tested during 10 RedOx cycles at 800 °C and one cycle at 850 °C.", "The OCV stayed constant over the cycles; the electrochemical performance dropped during the first utilization but was regenerated after a RedOx cycle and then stayed at the same value after multiple RedOx cycles (see Figure 27).", "The performance regeneration was believed to come from the creation of a porous Ni network stabilized by fine YSZ particles (see Figure 28) [186].", "Scale-up of the cell size to 48 cm2 active area was performed and tested over 40 RedOx cycles at 800 °C.", "The OCV decrease by about 1 mV per RedOx cycle whereas the electrochemical performance stabilized after 4 RedOx cycles [187].", "Conductivity measurements under RedOx cycling at 950 °C showed that coarse NiO-YSZ maintained high conductivity [126].", "Microstructure optimization showed that coarse NiO (keeping the same YSZ) enhanced the RedOx stability: after 10 RedOx cycles of more than 3 h at 850 °C, cell performances were stable at 0.7 Acm−2 at 0.7 V [165].", "Figure 27 OCV, current density (i) at 0.6 V and area specific resistance (ASR) of anode-support containing 60 wt % fine NiO, 38 wt % coarse and 2 wt % fine YSZ with the number of RedOx cycles (the last cycle is done at 850 °C).", "Conditions: 97% H2 + 3% H2O at 800 °C.", "Measurement done 1 h after re-reduction when not stated otherwise [186].", "Figure 28 Anode containing 60 wt % NiO after 300 h at 800 °C under humidified forming gas (10% H2 in N2) (a) and (c): fresh as-sintered sample, and (b) and (d): tested sample from Figure 27.", "The grey levels separate each phase (YSZ: light grey, Ni: dark grey and porosity: black).", "All data-bars are 2 μm in length [186].", "Nickel carbonate pyrolized at 500 °C or 700 °C is composed of agglomerates (dV50 = 10–15 μm) of very fine NiO particles (surface area between 13 and 46 m2/g).", "Anode supports of such NiO mixed with fine standard NiO (dV50 = 0.5 μm) and 3YSZ or 4ScSZ gave good RedOx stability (analyzed by electrical conductivity measurement) compared to only standard fine NiO and zirconia composite.", "With only nickel carbonate pyrolized-zirconia composite, the electrical conductivity was however low before RedOx testing [188]. 3.4.3.", "Sintering Temperature Lowering the sintering temperature from 1400 to 1100 °C seems to lower the damage in the YSZ skeleton and lowers the expansion from 0.6% to 0.1% after one RedOx cycle at 950 °C [66].", "Robert et al. also noted a higher irreversible expansion for higher sinter temperatures, but did not notice any other influence [185]. 3.4.4.", "Porosity Changing particle size and sintering temperature has a direct influence on the sample porosity.", "As the nickel expands to NiO, it is intuitive that an increase in porosity will let the nickel oxide fill the porosity without producing an expansion.", "This approach is proposed by Robert et al., where an optimized microstructure containing macro- and micro-pores limit the expansion during RedOx cycles [189].", "Pihlatie et al. observed that the increase in porosity decreased the expansion during RedOx cycles as shown in Figure 29 [73].", "A similar observation was reported for 46 different NiO-YSZ samples.", "Porosity higher than 45% in the as-sintered state should give RedOx stable supports with an expansion limit lower than 0.2%, but some samples with only 35% porosity also present low expansion (see Figure 30) [86].", "Figure 29 Maximum cumulative RedOx strain value (CRS) obtained after three isothermal cycles at 850 °C as a function of the total porosity of the Ni-YSZ composite [73].", "Inversely, Klemensø observed that low porosity is better for the RedOx stability as the strength of the support will be higher [27].", "Ettler et al. showed that when varying the gas flow (from 20 to 1200 ml/min) for a constant temperature (800 °C) and a constant time of oxidation (15 min), the degree of oxidation (DoO) of an anode support depends on its porosity.", "Samples with 48% porosity showed a DoO reaching 100% and cracking of the thin electrolyte whereas a denser support with 33% porosity only reached about 20% of DoO and presented no crack in the thin electrolyte [14].", "In this case, the limiting factor for oxidation is the gas diffusion process that is higher for the more porous sample.", "It should be noted that in practice, during air leakage or lack of fuel, the air flow will not vary so much but it will be more probable that time will vary and extend to longer periods.", "Figure 30 Expansion after one RedOx cycle at 800 °C versus porosity of 46 NiO-8YSZ anode-support samples [86]. 3.4.5.", "Composition The proportion between Ni and YSZ was studied by dilatometry on a fine microstructure: lowering the NiO content (from 57, 40, 35 to 30 wt %) seems to decrease the linear expansion between 57 and 35 wt %, but the 30 wt % sample had again a similar expansion than the 57 wt % sample [41].", "Inversely, based on coarse YSZ particle size, the expansion during RedOx cycles seems to be compensated by the large shrinkage during reduction for high NiO content samples [185].", "From ESC electrochemical tests, 40:60 vol % Ni:YSZ composition appeared to be more stable than 35:65 vol % under RedOx cycling [126].", "A statistical approach with 46 samples showed that the NiO content between 40 and 60 wt % does not have a significant effect on expansion during RedOx cycles [186].", "This can explain the contradictory results reported by different studies in this range of composition.", "In fact, at low NiO content (<30 wt %), decreasing the nickel content would limit the expansion over a RedOx cycle as shown by Wang et al.", "They studied Ni-YSZ composite sintered 6 h at 1400 °C with low amount of Ni (0 to 30 vol % Ni) for non-conductive substrates for segmented-in-series cells.", "Dilatometry measurements showed a RedOx stable behavior for concentrations of 10 vol % Ni (equal to 17.6 wt % NiO) or lower [190].", "In case of anode application, the electrical conductivity is essential.", "By lowering the nickel content, the electrical conductivity will dramatically decrease if the percolation threshold is violated (at 29.4 vol % for spherical particles with the same diameter [191]).", "Different strategies are proposed to decrease this threshold value. 3.4.6.", "Orientation and Particle Shape of Nickel Phase The particle shape and size of the electronic conducting phase change the percolation threshold.", "According to Maxwell’s theory, the relation between conductivity and particle shape can be found.", "Using metal particles with a larger axial ratio (M) and a smaller radius (r) reduces the minimum metal content required to reach a certain conductivity value.", "Xue performed metal-polymer experiments in good agreement with theory, with an electric threshold around 5% of metal particles of M = 6 and ellipsoid semi-radii of 1651, 275 and 275 nm, respectively [192] (see Figure 31).", "This idea has been recently patented for the zirconia particles shape [193].", "If the conducting phase could be organized, the percolation threshold could be decreased further.", "A way to organize the conducting phase is to put the tape-cast anode slurry in a magnetic field: as nickel and nickel oxide are ferromagnetic and antiferromagnetic, respectively, they will orient in the applied field [194].", "Magnetism measurements can also give the proportion between Ni and NiO [195] and the average size of the magnetic particles [196,197].", "Figure 31 Percolation threshold versus (a) axial ratio M and (b) radius of conducting particles r [192]. 3.4.7.", "Ni coated Pore-Former Graphite coated with Ni was used to produce Ni-YSZ anodes by tape-casting.", "The composite showed high conductivity with only 12 to 20 vol % of Ni (3–5 orders of magnitude higher than conventional anodes) [198,199,200,201,202]. 3.4.8.", "Ni Foam Corbin et al. proposed to use nickel foam impregnated with a mixture of Ni, YSZ and starch pore former in a polyvinyl alcohol solution.", "The samples were then sintered at 1475 °C in air for 1 h and finally reduced in dilute hydrogen at 1000 °C for 2 h [203,204].", "The electrical conductivity at room temperature shows that only 2 to 5 vol % of Ni (from the total volume including porosity) is needed to obtain more than 1000 S/cm compared to 10 vol % in the case of Ni coated graphite [202].", "Ni porous structure impregnated with Fe was used as a support for a complex cell using a La-doped ceria-Ni composite thin anode.", "A single RedOx cycle of 2 h at 700 °C presented a performance increase of about 1% at 0.27 W/cm2 [205,206]. 3.4.9.", "Wet Impregnation (WI) Wet impregnation uses dilute salts of active materials, which can be deposited inside a porous structure by a subsequent heat treatment, removing the organic material.", "This technique can be used to lower the quantity of expensive element or to avoid reaction between unstable components during sintering.", "A review on wet impregnation for SOFC application is compiled by Jiang [207].", "The limitation of this technique is the low mass loading per cycle, which means multiple thermal treatments are needed to obtain sufficient material.", "This represents a problem for upscaling the process.", "Jasinski et al. proposed to impregnate porous Sm0.2Ce0.8O2 produced by dry mixing with carbon powder (90:10 vol %).", "The porous substrate was impregnated with Ni nitrate to reach 7.5, 11 and 14 vol % Ni.", "The conductivity was tested over 10 RedOx cycles and seems stable around 80 S/cm for 11 vol % Ni.", "Measurement over time showed that the 14 vol % Ni reaches 80 S/cm after 100 h without change after a RedOx cycle [208].", "A similar approach was to infiltrate a porous YSZ skeleton by Ni nitrate salt (10 times with decomposition at 500 °C to obtain 12–16 wt % Ni).", "No expansion could be observed upon one RedOx cycle of 100 min at 800 °C.", "The room temperature conductivity is 360 S/cm and 290 S/cm after the RedOx cycle [117].", "Zhu et al. reported a RedOx stable YSZ skeleton support impregnated with nitrate solution including La3+, Sr2+, Cr3+, Fe3+ and Ni2+ ions and urea.", "The final impregnate anode is about 35 wt % LSCF-oxide and 5 wt % Ni.", "The cell gave stable performance of 0.5 A/cm2 at 0.42 V and 800 °C after 10 RedOx cycles between pO2 = 0.3 and a CH4/O2 ratio equal to 2.2 [209].", "Buyukaksoy et al. reported an electrolyte-supported cell with a 10 μm porous YSZ (sintered at 1150 °C) impregnated with nickel salt solution (loading about 30 vol % NiO after 20 cycles).", "The cell showed an activation upon the first 15 RedOx cycles at 800 °C, going from 0.8 to 1.5 A cm−2 at short circuit [210]. 3.4.10.", "Ni Coated Ceramic Impregnation was used to coat fine (0.3 μm) and coarse (10 μm) YSZ particles with NiO (40:60 vol % Ni:YSZ).", "The powders were uniaxially pressed as discs of 1.2 mm thickness.", "Thermo-RedOx cycles up to 800 °C under air were applied to the samples.", "Electrical conductivity decreased from 1450 to 1250 S/cm over 20 RedOx cycles, whereas for standard NiO-YSZ composites, the conductivity decreased from 1200 to 600 S/cm for the same treatment (due to higher Ni coarsening).", "The coated particles were used to produce anode supported cells with an electrochemical performance of 0.56 W/cm2 at 800 °C and 0.5 V [211].", "A similar process was used to coat NiO on YSZ and CGO.", "Composites made of 35:65 wt % YSZ:NiO and CGO:NiO showed high strength of 241 MPa and 146 MPa and high electrical conductivity of 2890 and 2710 S/cm, respectively [212]. 3.4.11.", "Graded Composition and Porosity (1) Anode functional layer The use of a graded content of Ni and porosity in the AFL showed an improvement in the RedOx stability of the anode as Waldbillig et al. demonstrated in a recent paper [213].", "The RedOx sensitivity of the cell after a full cycle for the graded AFL is only half that of the standard one.", "This approach is also considered by Bloom Energy® on ESC technology but with a gradient along the cell length and the anode thickness.", "This study was based on anode graded composition of Ni and Ce0.8Sm0.2O2 (SDC) done by ink jet printing (higher content of SDC close to the entrance of the fuel and close to the anode-electrolyte interface).", "The cells were compared to standard cells in a 10 cells stack configuration.", "The oxidation was performed under constant temperature and constant current load by decreasing the fuel flow to zero in about 5 h.", "After the first RedOx cycle, the Rs and Rp were compared between the different cells, showing an Rs increase of 24% for standard cells and only 3% for the new cells.", "The Rp increased by 22% for standard cells and decreased by 1% for modified cells.", "After the second RedOx cycle, the overall Rs increase for the new cells was 5% and 1% for Rp [132]. (2) Anode support A graded support was fabricated by slip casting using water-based slurry.", "The porosity gradient permitted to lower the porosity down to 30% without having too much diffusion limitation through the 0.8 mm thickness of the support.", "These supports could reach 39% electrical efficiency at 250 mW/cm2, 0.65 V and 850 °C in a Hexis stack.", "After a RedOx cycle at 920 °C, the OCV decreased from 990 to 850 mV, showing the limitation of this anode support at this temperature [90].", "A similar approach was taken by Ihringer et al. who produced anode supports of thickness from 0.3 to 1.2 mm with lower amount of nickel (addition of starch pore former was used to increase porosity) [105].", "The electrochemical tests on 1 cm2 gave initial power density of 0.98 W/cm2 and a final one of 0.7 W/cm2 after 10 RedOx cycles at 800 °C and 0.7 V.", "Repeat element configuration with a 44 cm2 active surface shows a constant OCV and a small decrease of potential from 0.89 to 0.87 V at 0.23 A/cm2 and 800 °C after 10 RedOx cycles, 2 thermal cycles and 400 h of utilization.", "The mechanical strength of these supports increases slightly from 145 to 155 MPa after 10 RedOx cycles (the Weibull modulus also increases from 6 to 9) [214].", "Further studies showed 75% of Fu and 42% of electrical efficiency (at 0.38 W/cm2, 0.7 V and 806 °C) [181].", "A recent study on a single repeating unit stack of 100 cm2 active area (based on Hexis design) tested over 1700 h and 16 full RedOx cycles (more than one hour under air at 800 °C) gave a powder degradation (at 0.25 A/cm2) of 0.3% per cycle.", "The OCV dropped about 40 to 50 mV during the measurement (see Figure 32) [215].", "Figure 32 Anode supported cell tested over 16 RedOx cycles and 1700 h on a single repeat unit stack configuration.", "Test conditions: 800 °C, active surface area about 100 cm2 and constant current load of 0.25 A/cm2 [215]. 3.4.12.", "Controlled RedOx Cycle As RedOx cycles change the sample microstructure, it was proposed to apply to the anode support a controlled RedOx cycle to enhance the RedOx stability.", "Wood et al. observed a lower decrease in performances on preconditioned samples (one RedOx at 550 °C) with only 3.2% decrease in voltage at 0.75 A/cm2 after a RedOx cycle at 750 °C compared to 10.8% decrease without the preconditioning.", "There are several stages in the fabrication where the initial controlled RedOx cycle may be applied.", "It can be done on the mixture prior to the formation of the green anode structure, then on the fired sample before insertion in the stack and finally, in situ in the stack [216].", "Pihlatie et al. showed an increase of electrochemical performance after a RedOx cycle at 650 °C in a symmetrical cell configuration [73].", "Different groups observed an increase in performance over short-term RedOx cycles [175,213].", "This is believed to be due to the enhancement of the contacting layer at the anode side. 3.5.", "Alternative Anode Materials 3.5.1.", "Alloys and Additives for Metal-Ceramic Anode A potential solution is to use an alloy (or even noble metal) with higher oxidation resistance.", "The idea is to slow down the kinetics [145], make a protective layer on the nickel [145] or limit the nickel coarsening [189,217].", "The addition of noble metal particles in the anode was presented by Huang et al. [160].", "The idea was to cover the metallic phase by nanoparticles of oxide (YSZ, ScSZ, CGO, CeSmO, LSGM) to reduce vapor loss and agglomeration of noble metal particles.", "The proportion of the anode was around a third of each phase, metallic, ceramic and porosity.", "Some results are shown over two RedOx cycles with an ESC and CSC configuration, but the main limitation of the approach is the price of the noble metal.", "Several authors alloyed copper with nickel [218,219,220,221,222].", "The aim of Cu addition, usually coupled with a ceria-based ceramic, is more to limit hydrocarbon cracking than to enhance RedOx stability of the anode, but RedOx cycles have been tested at 750 °C under methane/air and shown slow regeneration over 100 h to reach initial performance [220].", "Robert et al. proposed the addition of a doping element such as Al2O3, TiO2, CeO2, MgO or spinel compounds and salt or oxide from Ni, Mn, Fe, Co and Cu as sintering aids and MgO as inhibitor of nickel grain growth [189], to prevent RedOx instability of the Ni-YSZ anode support.", "The addition of CeO2 had already been proposed earlier by researchers from the Dornier Research Center [223,224] with apparently promising results but unfortunately very little published results.", "Larsen et al. proposed to add another oxide to the anode (Cr2O3, TiO2, Sc2O3 , Al2O3, VOx, TaOx, MgCr2O4, CaO, MnOx, Bi2O3, LnOx NbOx, ...) [217].", "The claim is to prevent nickel coarsening due to Ni-particle growth inhibitors, to surface passivate the Ni, to slow down the kinetics of oxidation and to strengthen the ceramic structure of the anode support and/or anode layer.", "The author tested the addition of 5 wt % of Cr2O3 in the anode support and observed formation of NiCr2O4 during sintering and the reduction of this phase resulted in a partial surface coverage of Ni particles that stabilizes the structure.", "The addition of 7 wt % TiO2 in the active anode layer forms NiTi2O4 that creates small particles of TiO2 after reduction of the anode.", "These particles prevent Ni particles from coarsening.", "The use of Cr2O3, TiO2, Sc2O3, Al2O3 decreases the anode thermal expansion coefficient.", "Addition of equal molar amounts of NiTiO3 and (Sr,La)ZrO3 gives a composite of (Sr,La)TiO3, NiO and ZrO2 after sintering.", "After reduction the microstructure provides catalytic activity as well as electronic conductivity [217].", "Jain et al. proposed to use a natural stone as sintering aid (Dolomite, D): CaCO3 + MgCO3 + impurities (CaO 66.2%, MgO 32.3%, Al2O3, Na2O 0.34%, SiO2 0.26%).", "This shows an increase in strength (maybe due to a decrease in porosity).", "Comparable electrochemical performances were presented with 2 wt % addition.", "No RedOx tests were shown in this study [225].", "From alloy corrosion, it is known that a small addition of solute can increase the oxidation rate of Ni [46], but above a certain level (5 at %) a passive layer can be formed (e.g., of Cr2O3 or Al2O3,) depending on composition, which slows down or stops the oxidation [25] (see Section 2.2.2).", "A kinetic study compared the addition of MgO, TiO2 and CaO (4 mol % in a 40:60 vol % YSZ:NiO) to a pure composite [36].", "All dopants slow down the oxidation rate between 650 and 800 °C, the most efficient being CaO.", "The microstructures with dopant present less porosity, which could be due to a decrease of the Ni2+ diffusion along the NiO grain boundaries.", "Another kinetic study based on thermogravimetric analysis (TGA) presents the addition of 1, 3, 5 and 10 mol % of Al and Ce to NiO (by nitrate salt addition).", "After homogenization with YSZ and sintering for 2 h at 1450 °C, the samples were crushed before being measured in the TGA.", "The results showed that the additives increased both the rate of reduction under dilute hydrogen and the rate of oxidation under air at 800 °C.", "Even if the additives are different, the results are not consistent with Tikekar’s study [36] but correlate better with the results on alloys [46].", "This discrepancy could be linked to microstructural differences; grain boundary diffusion of Ni2+ should be lower but a decrease of the NiO grain size could again increase the oxidation rate.", "Expansion measurements showed that NiO doped with Ce (sintered around 1360 °C) presented maximal strain smaller than 0.1% during 3 RedOx cycles at 850 °C, compared to undoped NiO with a value between 0.2% and 0.3% [73].", "Doping with Al2O3 gave 0.22% expansion.", "With MgO, the first RedOx cycle induced a significant expansion of 0.35%, the following cycles only 0.14%.", "Ceria could thus be an option to further lower the ASC expansion.", "Another study based on in situ curvature measurements on half-cells showed that 5 mol % of Ce in NiO bent the anode towards the electrolyte during reduction, due to the expansion of cerium in reducing atmosphere (cracks occurred in the thin electrolyte).", "Undoped samples bent towards the anode as usually observed [100].", "Previous results reported by Klemensø presented an initial increase in length during reduction at 1000 °C of 0.7% for a composite based on 55 vol % NiO, 26 vol % 3YSZ and 19 vol % CeO2 [27].", "The better additive is found to be 13.5 vol % of Al2O3 (with 51 vol % NiO and the rest 3YSZ), leading to 0.28% of strain during expansion at 1000 °C (compared to 0.35% for the undoped sample).", "Addition of 20 vol % TiO2 seems not beneficial, with more that 2% strain measured on a RedOx cycle.", "These two last studies are inconsistent with Pihlatie et al. as he observed a strong shrinkage (of 0.2%–0.3%) during reduction of the Ce doped samples [73].", "The difference probably again stems from the difference in composition, microstructure and porosity of the samples.", "It is possible that by optimization the right proportion of NiO and CeO2 can be found, where the volume changes of the two phases can compensate each other during reduction and oxidation.", "In a different study, TiO2 seems beneficial against RedOx cycles [226].", "Two compositions containing 1 wt % TiO2 were prepared as follows: (1) Nickel chloride hydrate and titanium tetrachloride (combustion method) mixed with 10Sc1CeSZ and (2) standard powder mixture of TiO2 and NiO.", "A RedOx cycle at 1000 °C in air resulted in a linear expansion of 0% and 0.04%, respectively (without TiO2: 0.34% and 0.31%, respectively).", "A RedOx stability test at 800 °C was performed on Cu-LSCM (La0.75Sr0.25Cr0.5Mn0.5O3−d) pellets by four-point electrical conductivity measurement giving promising results [227].", "(Mg,Ni)O (65:35 in mol %) solid solution showed an expansion under the first reduction of 30 h (of about 1%) and a shrinkage of 0.4% upon reoxidation [228].", "The second reduction during 220 h induced a strong expansion of 3.5%.", "This is correlated to the exsolution of Ni separated to the grain boundaries of MgO (small particles of Ni were observed at the surface of MgO grains).", "This effect could be used to compensate the expansion of pure Ni during oxidation but Pihlatie et al. did not observe this effect adding a small amount of Mg to NiO [73].", "Application of similar compounds was presented by Fujita et al. for a segmented-in-series SOFC substrate based on Ni-doped MgO with 8YSZ produced by extrusion.", "They showed partial RedOx cycles without electrochemical degradation [178].", "Later, the same group compared the stress build up in NiO-YSZ and NiO-MgO-YSZ composite during RedOx cycles using the XRD technique; the compressive stresses in the thin YSZ electrolyte strongly decreased with NiO-YSZ whereas it stayed constant with MgO [229].", "Dilatometry and residual stress in the electrolyte measurement showed a RedOx stable behavior at 800 °C of NiO-MgO-YSZ composite from 5 to 30 vol % NiO [230].", "The addition of a stable oxide in nickel RedOx cycling was also studied for chemical looping combustion applications [231,232].", "From this short overview on additives to Ni-YSZ anode for RedOx stability enhancement, it is not clear whether this strategy can be successful.", "The effects of these additives appear at any stage from fabrication to reduction and reoxidation.", "They will change the microstructure of the composite and of NiO by producing spinels like NiCr2O4 or NiAl2O4 and other compounds that can lower the sintering temperature. 3.5.2.", "Full Ceramic Anode This sub-section could be a full subject on its own.", "Here, only main results will be given.", "Ceramic anodes are considered to overcome the limitations of Ni based anodes, which are cracking of hydrocarbon fuel, poisoning with sulfur and other species, and limited RedOx stability.", "A general review for ceramic anodes is available in [233], another is specific on RedOx stability of ceramic based anodes [15].", "The principal needs for ceramic anodes are [234]: Negligible dimensional change during RedOx cycles (less than 0.1 to 0.2% of linear expansion).", "Electrical conductivity higher than 10 S/cm.", "Stability in reducing atmosphere and air and compatibility with the electrolyte.", "Thermal expansion coefficient close to that of the electrolyte.", "In case of YSZ: between 10 and 11 × 10−6 K−1.", "Good catalytic activity for H2 and CH4 oxidation.", "In case of mixed conductivity the ionic conductivity should be >0.02 S/cm.", "Fu et al. proposed to separate the support from the active ceramic anode functions [15].", "Where only the active layer must possess electrocatalytic activity and good ionic conductivity, the support needs high electrical conductivity.", "According to Table 7, the best candidates could be ZrTiYO2, LaSrCrMnO3, SrYTiO3 and LaSrTiO3. membranes-02-00585-t007_Table 7 Table 7 Summary of properties of some potential oxide anodes at 800 °C under reducing conditions [235].", "Materials CTE (10−6 K−1) Electronic conductivity (S/cm) Ionic conductivity (S/cm) Polarization resistance RedOx stability CeO2 12 0.5–1 0.1–0.2 ++ – ZrTiY-oxide 10 0.1 0.01 + ++ LaSrCrRu-oxide 10 0.6 small ++ + LaSrFeCr-oxide 12 0.5 ?", "++ + LaSrCrMn-oxide 10 3 ?", "+++ ++ LaSrCrV-oxide 10 ?", "?", "++ ++ SrYTi-oxide 11–12 80 small + +++ LaSrTi-oxide 10 40 small ++ +++ Nb2TiO7 1–2 200 very small – – GdTiMoMn-oxide ?", "0.1 reasonable + – BaCe0.8Y0.2O3 ?", "0.02 ?", "– ++ The first paper on a full ceramic anode that shows RedOx stability was proposed in 1999 by Marina et al.", "The configuration was ESC of 180 μm thickness (8YSZ) and an anode of 8YSZ (anchoring layer made of coarse particles) and 40CGO sprayed 15 μm thick.", "A power density of 470 mW/cm2 was obtained at 1000 °C and 0.7 V in 9% H2.", "Several RedOx cycles were carried out by turning off the fuel gas and letting the OCV drop to 0 V without any degradation [236].", "In a later study, LaxSr1−xTiO3 presented high electrical conductivity for samples sintered under H2. 14 RedOx cycles at 500 °C (overnight) caused a 40% decrease in conductivity, and then only 10 to 24 min per further RedOx cycle led to a final conductivity of 300 S/cm.", "The expansion was lower than 0.1% during RedOx cycles at 1000 °C.", "The good initial performance decreased rapidly after the RedOx cycles to only about 60 mA/cm2 [237,238].", "Strontium titanates have been studied by several groups, because of their high electrical conductivity and dimensional stability under RedOx treatment.", "SrTiO3 doped with Y, Sc, La and cerium oxide doped with Nb, V, Sb and Ta were patented as ceramic anode to work in SOFC and solid oxide electrolyzer cell (SOEC) mode.", "The expansion during a RedOx cycle was lower than 0.1% [239,240].", "A parallel patent proposed SrTiO3 doped with Y, La, Gd that shows expansion during RedOx cycles lower than 0.14% and a polarization resistance lower than 0.3 Ohm cm2 at 800 °C when infiltrated by Ni [241].", "More recently Miller and Irvine proposed a study changing the B-site of La0.33Sr0.67Ti0.98X0.08O3 with X = Al3+, Ga3+, Fen+, Mg2+, Mnn+, Sc3+.", "During TGA measurements, Mg showed the lowest amount of reoxidation strain in air up to 900 °C: +0.11% < Sc (0.14%) < Al (0.16%).", "Conductivity was higher for Ti (8 S/cm) > Al > Ga and the performances were better in case of Ti (0.32 A/cm2 at short circuit) > Mn (0.3 A/cm2) > Ga (0.26 A/cm2) > Al (0.25 A/cm2) [242].", "Gross et al. developed a ceramic anode with high performance (850 mW/cm2 at 800 °C), composed of a thin active functional layer (AFL) on a non-catalytic conductive layer [243].", "The AFL composition was 1 wt % Pd, 40 wt % ceria in YSZ.", "The support was based on La0.3Sr0.7TiO3 (LST).", "La0.2Sr0.8Cr0.8Pd0.2O3−d-10GDC anode on LSGM (La0.8Sr0.2Ga0.8Mg0.2O3−d) electrolyte-support presented good electrochemical performance (0.47 W/cm2 at 0.6 A/cm2 and 800 °C) followed by 20% degradation over 200 h.", "After RedOx cycling at 800 °C, the performance regenerated probably due to Pd-nanoparticles re-nucleation during RedOx cycling [244].", "Different papers propose the use of (La0.75Sr0.25)1−xCr0.5Mn0.5O3 (LSCM) as anode and cathode materials for a RedOx-stable symmetrical SOFC [245,246,247].", "Barnett et al. showed that LSCM (47.5 wt %) with CGO (47.5 wt %) and NiO (5 wt %) anode yields relatively good performance under CH4 with 150 mW/cm2 at 750 °C, activating during 4 RedOx cycles of 30 min under air (shown in Figure 33) [248].", "Similar results are shown for (La0.8,Sr0.2)(Cr0.98,V0.02)3/CGO/NiO and (Sr0.86,Y0.08)TiO3/CGO/NiO anodes [248,249].", "Recently, Cassidy et al. reported the integration of the LSCM anode in the Rolls-Royce IP-SOFC concept, the power density is relatively low with 75 mW/cm2 [250].", "Martinez-Arias et al. showed the possible application of a cerium-terbium based anode for SOFC [251].", "Tomita et al. described the RedOx stability of a BaCe0.8Y0.2O3 anode but the power density is very low [252].", "Ca- and Co-doped yttrium chromite and samaria-doped ceria (SDC) composite anode in a ESC configuration was tested under multiple RedOx cycles at 800 °C without degradation due to its chemically and dimensionally stable behavior [253].", "Strontium molybdate (SrMoO4)-YSZ composite with 1 vol % Pd catalyst appears stable after a RedOx cycle at 800 °C and gave a relatively good performance of 0.3 W/cm2 [254].", "Figure 33 (La0.75Sr0.25)1−xCr0.5Mn0.5O3 (LSCM) (47.5 wt %) + CGO (47.5 wt %) + NiO (5 wt %) under CH4 with 150 mW/cm2 at 750 °C before and after RedOx cycles [248].", "The Forschungszentrum Jülich has studied the doping of strontium titanate as SOFC anode for many years [15,234,241,255,256,257,258,259].", "Recently, a breakthrough for a ceramic anode supported cell with high performance and RedOx stability was achieved with a Sr0.895Y0.07TiO3 (SYT) support, a (Sr0.89Y0.07)0.91TiO2.91-YSZ anode impregnated with 3 wt % NiO, and the YSZ electrolyte protected with a thin 20GDC interlayer so as not to react with a LSC cathode [260,261].", "A current density of 1.5 A/cm2 at 800 °C and 0.7 V was obtained.", "The OCV decreased only by 1% over 200 RedOx cycles (of 10 min in H2 and 10 min in air) at 750 °C, whereas the current density lowered by about 40% during the 200 RedOx cycles (see Figure 34) [260,261].", "A more recent study showed that the same cell tested in [260,261] had an OCV decrease of 5% after two RedOx cycles of 5 h under air at 750 °C (compared to the previous cycles of only 10 min under air).", "Interestingly, the performance reactivated after these cycles, which could be due to hot spots at the thin electrolyte cracks [262].", "Figure 34 Open circuit voltage (open circle), current density at 0.7 V (10 min in H2 and 10 min in air) at 750 °C (closed circles), and current density at 800°C applying 2 h in H2 and 10 min in air (closed square), all as a function of the number of RedOx cycles with SYT ceramic anodes [260,261]. 3.5.3.", "Mechanically Stronger Materials By increasing the fracture strength of mechanical support materials, fewer cracks will appear after a RedOx cycle.", "Klemensø et al. used this approach to find a more RedOx stable anode-supported cell [26,28].", "They used 3YSZ in the anode support instead of 8YSZ as the former’s bending strength is four times higher than the latter’s.", "The addition of about 1 wt % of Al2O3 further enhanced the strength of the support.", "The addition of YSZ or high strength material fiber can increase the strength of the anode support.", "The fibers should be co-fired with smaller YSZ particles. 3.5.4.", "Use Support with Higher Thermal Expansion Coefficient (TEC) Robert et al. observed better RedOx stability with higher NiO content.", "A possible reason for the better stability is the larger electrolyte compression stress [185].", "The maximal strain accepted from the electrolyte is 0.04% without residual stress of the electrolyte.", "By including a compressive residual stress of 240 MPa in the electrolyte after firing, the maximal strain increased to 0.17%, as described by Klemensø [28].", "If the compressive stress reaches 440 MPa, the maximal strain can be improved at least to 0.3%.", "The electrolyte can be put artificially under compression using a higher TEC support.", "The important point will then be thermal cycling stability and the stacking of these cells that will present higher curvature. 3.6.", "Kinetics 3.6.1.", "Oxidation Barrier Applying a nickel-rich layer on the anode support (opposite to the electrolyte) may stop oxygen diffusion to the anode.", "As the nickel-rich layer oxidizes first, the porosity closes and the oxygen diffuses slowly to the RedOx sensitive ALF.", "At 750 °C, it takes almost twice the time to reach the same degradation with the oxidation barrier compared to the standard cell [143,263].", "This extra time could allow the cooling of the system to a safe temperature, preventing RedOx degradation. 3.6.2.", "Improved Sealing The idea is to block fuel gases into the anode compartment with valves during stack cooling.", "This requires efficient sealing, like glass-ceramics, to prevent any leakage.", "Versa Power Systems tested their standard cell by closing the inlet and outlet of the anode during 15 h at 750 °C and no degradation was observed [143]. 3.6.3.", "Lower Operating Temperature The decrease of operating temperature down to 700 °C will strongly reduce the reoxidation kinetics and maybe limit the RedOx problem.", "Using scandium-stabilized zirconia (ScSZ) for electrolyte will decrease the ohmic loss due to lower ionic conductivity of YSZ at low temperature [264].", "Toho Gas built a 1 kW stack based on ScSZ electrolyte [265].", "Ni-Fe anode substrate with La0.73Sr0.1Ga0.64Mg0.26O3−d (LSGM) electrolyte and Sm0.4Sr0.6Co1.6O3−d (SSC) cathode gave 0.16 W cm−2 at 673K with RedOx stability for 2 cycles (2 h under oxidizing atmosphere) [266].", "Scale-up of this technology still remains to be achieved.", "The main limitation at low temperature will come from the cathode activity for oxygen reduction. 4.", "Synthesis for Ni-Based Anode-Supported Cells Based on the literature review of the RedOx instability of standard anode-supported cells given in Section 2, Figure 35 summarizes the major trends.", "In this scheme, the electrolyte is supported by the anode, where sintered grains are represented by circles.", "During the reduction, the porosity increases due to the volume reduction of about 41% of nickel oxide to metallic nickel.", "From this state, the standard half-cell can be subjected to three different treatments: (1) reoxidation at low temperature (600–700 °C, Figure 35d); (2) utilization of the half-cell with nickel coarsening (Figure 35c) and reoxidation at low temperature (Figure 35e) or (3) reoxidation at higher temperature (800–1000 °C, Figure 35f).", "Figure 35 Scheme of RedOx instability of standard anode supported Ni-YSZ half-cell [129].", "At low temperature (case 1), nickel reoxidation is homogeneous through the whole anode support layer due to the faster gas diffusion compared to solid-state diffusion.", "The nickel oxide presents fine closed porosity created by the outward diffusion of Ni2+ through the nickel oxide grain boundaries during oxidation.", "Due to the closed porosity, the volume difference between reoxidized and as-sintered nickel oxide is positive.", "This induces a volume increase of the anode support and therefore tensile stresses and cracks in the thin electrolyte.", "During utilization (case 2), the nickel phase reorganizes to lower its surface energy.", "Nickel coarsening will be halted by the zirconia backbone after a few hundreds of hours.", "If reoxidation occurs after Ni coarsening, the net volume increase of nickel oxide should be similar to the one without utilization.", "But due to the reorganization of the nickel phase inside the composite, its volume increase could be higher because of the creation of porosity between the nickel oxide and zirconia phase.", "The higher linear expansion of the anode support after coarsening was confirmed by Pihlatie et al. [72].", "The effect of temperature on the RedOx instability of Ni-YSZ anode-supported cells is more important compared to nickel coarsening.", "During oxidation at high temperature (800–1000 °C) (case 3) without previous utilization, the kinetics of solid-state diffusion is faster than gas diffusion, which induces an inhomogeneous oxidation and a sharp reduced/oxidized interface in the composite.", "This will develop high stresses and non-linear deformation inside the anode support.", "The composite creep creates bending of the cell towards the anode.", "First, at higher temperature, the porosity of the reoxidized nickel is coarser.", "The self-diffusion of nickel cation changes from shortcut-path-controlled to crystal-lattice-controlled between 700 and 1000 °C [47].", "This can have an influence on the NiO internal porosity.", "Second, cracks in the YSZ backbone are observed and located at the zirconia grain boundaries due to higher diffusion at this location.", "These two effects make the linear expansion of the anode composite increase at high temperature.", "The higher volume expansion and the bending effect are cumulated and create higher crack density of the thin electrolyte.", "As described in the general discussion, the Ni-YSZ anode-support microstructure can be modified to enhance its RedOx stability.", "The key measure is the porosity increase, to allow more space for the nickel oxide volume increase during RedOx cycles.", "This could be achieved by pore-former addition and using coarser zirconia particles.", "Figure 36 schematically depicts the behavior of an anode support optimized for RedOx stability during utilization and multiple RedOx cycles (as well as micrographs shown in Figure 28).", "An optimized microstructure includes fine nickel oxide to enhance the electrical conductivity, coarse zirconia to increase the porosity and a small addition of fine zirconia needed for sintering and stabilizing the microstructure.", "During first utilization, the performance and the electrical conductivity drop rapidly because of important coarsening of the conductive phase (Figure 36).", "The RedOx optimal microstructure has wider voids in the YSZ backbone, which means the nickel phase can reach coarser sizes.", "In addition, as the porosity is higher, the conductivity is lower.", "After multiple RedOx cycles, the electrolyte does not show cracks thanks to the low volume expansion of the highly porous support.", "A NiO internal porosity similar to that in the standard anode-microstructure is observed after RedOx cycles.", "But this internal porosity remains unchanged during reduction and during utilization due to fine zirconia particle encapsulation during the multiple RedOx cycles.", "The nickel volume is equal but, as it contains stable porosity and fine zirconia particles, its connectivity within the anode is increased compared to the microstructure after first utilization.", "Figure 36 Scheme of RedOx behavior of highly porous Ni-YSZ anode supported half-cell [129].", "High porosity decreases strength and conductivity [86,93,186,267].", "Yet an anode support of optimal porosity and composition should retain sufficient mechanical properties, electrical conductivity and RedOx stability.", "As described through the different scales reviewed in this work (from nano to macrostructure), the key issue for RedOx stability is porosity.", "Optimal compositions of RedOx stable anodes contained between 47% and 52% of porosity [86].", "On the other hand, porosity will decrease electrical conductivity and mechanical strength of the Ni-YSZ composite.", "Hence an optimal porosity should be determined to achieve a RedOx stable, highly conductive and strong anode support.", "Figure 37 depicts the central role of porosity in the Ni-YSZ anode support properties.", "The conductivity could be increased by adding more nickel and by changing the shape of the nickel (foam, coated pore-former or ceramics [201,202,204]).", "To enhance mechanical stability (maximal force at rupture), the thickness of the anode support should be increased.", "Figure 37 The central role of porosity in the Ni-YSZ anode supported solid oxide fuel cells properties. 5.", "Conclusions The key advantage of fuel cells is their high efficiency for converting chemical energy from a variety of fuels directly into electricity.", "Solid oxide fuel cells (SOFCs) are among the most interesting fuel cells technologies due to the highest efficiencies achievable even for small systems, to their ability for co-generation (heat and electricity) and to their feedability with many hydrocarbon-based fuels with manageable pretreatment or cleaning.", "Current SOFC limitations remain a certain fragility of the components, the high cost of some materials and the performance degradation at operating temperature.", "Reduction and oxidation (RedOx cycle) of the Ni-YSZ anode at high temperature can decrease dramatically the performance of SOFC, especially for anode-supported cell designs.", "The volume increase during nickel oxidation induces tensile stress and cracks in the thin electrolyte.", "The irreversibility of the RedOx cycle is due to different causes: (1) The internal porosity of NiO increases after reoxidation.", "The oxidation is governed by cationic diffusion: Outward diffusion of Ni2+ creates pseudo-Kirkendall porosity within the NiO particles. (2) The nickel coarsening during anode utilization creates a rearrangement of the phase.", "During reoxidation NiO does not reoccupy its original sites.", "Water vapor presence increases coarsening of the nickel phase. (3) Higher temperature (>700 °C) induces inhomogeneous oxidation (only the outer surface layer is oxidized) that produces bending of the cell.", "This can increase the stress in the thin electrolyte. (4) Low partial pressure of oxygen and high water vapor pressure induce inhomogeneous oxidation similar to the one described under (3).", "Solutions proposed in the literature are summarized in Figure 22.", "These solutions can be separated in two main families: (i) system and (ii) material solutions.", "To reach a RedOx stable system, the two families could be used in conjunction.", "System solutions suit large systems better while material solutions can be used for any system size.", "For the material solutions, the main routes are variations in: (a) stack design, (b) cell design, (c) materials choice, (d) Ni alloying, (e) kinetics of oxidation and (f) microstructure of the Ni-ceramic composite.", "All of these directions are potentially interesting.", "To reach a RedOx stable microstructure keeping a Ni-ceramic composite, the following aspects can be optimized: (1) Porosity enhancement. (2) Graded composition with more YSZ close to the electrolyte and the gas outlet to reach higher fuel utilization. (3) Particle size and particle size ratio between NiO and YSZ.", "Coarse microstructures are more RedOx stable. (4) Lower sintering temperature. (5) Ni foam and Ni-coated pore-former and ceramic phase. (6) Ni wet impregnation of the ceramic skeleton.", "The important drawback of this technique is the multiple impregnation and calcination cycles needed to reach even then only a few wt % of impregnated Ni.", "All these microstructure changes to reach RedOx stability, especially the increase in porosity, should be considered in the light of other needs of the anode and the cell.", "The support and the anode composition can be modified.", "For the anode support, the optimal microstructure should have a good conductivity, a low expansion during RedOx cycles and a high strength.", "For the anode active layer, the optimal microstructure should possess a good electrochemical activity for fuel oxidation and a relative low expansion during RedOx cycles.", "Finally, the optimal solution for RedOx instability of the solid oxide fuel cells anode will be a conjunction of different solutions at multiple levels of the SOFC module.", "Before building a SOFC system, the cost for RedOx instability solutions versus total cost should be evaluated.", "This will depend on the system size and its utilization mode.", "For large stationary modules, the system solution would be the first choice (including a secondary solution like cell-design, for example); for a small mobile module (like auxiliary power unit, APU), the solution is a combination of stack-design, cell-design, material choice and microstructure optimization.", "A RedOx stable system could for example be based on a good electrically conductive porous support (like doped SrTi-oxide or high temperature stainless steel) with a thin porous ceramic layer (like SmCe-oxide or doped YZr-oxide) impregnated with electrochemical active particles (like Ni and Ce-oxide).", "The dense thin electrolyte could be LaSrGaMg-oxide or standard stabilized-zirconia.", "A low temperature active cathode (like LaSrCoFe-oxide or SmSrCo-oxide) can be used, together with an interlayer against diffusion or reaction for long term stability.", "RedOx stability is still only one requirement of a good anode and anode-support.", "The optimal anode should have a coefficient of thermal expansion similar to other stack components, display high electrochemical activity for hydrogen, CO and hydrocarbon fuel oxidation and be chemically stable with respect to the other stack components.", "The stability over time (i.e., no change in microstructure), with hydrocarbon fuels and with impurities like sulfur, phosphorus and others, is also essential.", "All these requirements should be fulfilled in order to obtain the optimal solid oxide fuel cells anode. 6." ]

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[ "Nanocrystalline ceria coatings on solid oxide fuel cell anodes: the role of organic surfactant pretreatments on coating microstructures and sulfur tolerance Nanocrystalline ceria coatings on solid oxide fuel cell anodes: the role of organic surfactant pretreatments on coating microstructures and sulfur tolerance WuChieh-Chun1TangLing1De GuireMark R1 SteinemClaudia Guest EditorBillJoachim Guest Editor 1Department of Materials Science and Engineering, Case Western Reserve University, 10900 Euclid Avenue, Cleveland, Ohio, 44106-7204, USA10.3762/bjnano.5.181 Summary Treatments with organic surfactants, followed by the deposition of nanocrystalline ceria coatings from aqueous solution, were applied to anodes of solid oxide fuel cells.", "The cells were then operated in hydrogen/nitrogen fuel streams with H2S contents ranging from 0 to 500 ppm.", "Two surfactant treatments were studied: immersion in dodecanethiol, and a multi-step conversion of a siloxy-anchored alkyl bromide to a sulfonate functionality.", "The ceria coatings deposited after the thiol pretreatment, and on anodes with no pretreatment, were continuous and uniform, with thicknesses of 60–170 nm and 100–140 nm, respectively, and those cells exhibited better lifetime performance and sulfur tolerance compared to cells with untreated anodes and anodes with ceria coatings deposited after the sulfonate pretreatment.", "Possible explanations for the effects of the treatments on the structure of the coatings, and for the effects of the coatings on the performance of the cells, are discussed. cerium(IV) oxide microstructure organic self-assembled monolayers solid oxide fuel cells sulfur tolerance This article is part of the Thematic Series \"Towards multifunctional inorganic materials: biopolymeric templates\".", "Introduction Fuel cells convert chemical energy directly to electrical energy.", "Compared to conventional power sources, fuel cells offer higher efficiencies, lower emissions, modular installation scalable from milliwatts to megawatts, and distributed power generation to reduce transmission losses [1].", "Among fuel cell technologies, solid oxide fuel cells (SOFCs) offer unique benefits [1–2].", "They run not only on hydrogen, but also on widely available hydrocarbon fuels.", "They need little or no precious-metal catalysts.", "They provide high-quality utility-grade heat, which in combination with electrical efficiencies of up to 60% leads to total system efficiencies of 80–85%, exceeding conventional power sources.", "SOFCs thus have tremendous potential to meet rising global demand for electrical energy more efficiently and with lower environmental impact than conventional power sources.", "A fuel cell consists of a dense ionically conducting layer (electrolyte) with porous electronically conducting layers (the electrodes) on each side, separating the fuel (e.g., H2) from its oxidant (typically O2 in air).", "In typical solid oxide fuel cells (SOFCs), oxygen molecules are reduced to oxide ions at the air electrode (the cathode) by electrons from the external circuit.", "The oxide ions cross the electrolyte and combine with H2 at the fuel electrode (the anode, the focus of the present study) to form H2O, releasing electrons into an external circuit to do electrical work before they pass to the cathode for consumption in the oxygen reduction reaction.", "It is well known that the performance of SOFC anodes, typically composites of nickel metal with a zirconia or ceria ionic conductor, is degraded by sulfur impurities in the fuel, severely reducing both the power generated by the cell and its operating lifetime.", "(For recent reviews, see [3–4].)", "The extent and permanence of this “sulfur poisoning” varies with operating temperature, current density, sulfur concentration (as low as a few ppm), and anode materials [5–12].", "Current consensus holds that adsorption of sulfur onto the nickel surface [13] may impede the ability of nickel to catalyze the oxidation of hydrogen [9,14–16].", "Understanding sulfur poisoning is crucial to developing SOFCs that could operate on commercial, sulfur-containing hydrocarbon fuels (such as diesel and aeronautical fuels) and fuels derived from sulfur-containing sources such as coal.", "Studies [17–21] have shown that incorporating ceria into the anode, either to replace yttria-stabilized zirconia (YSZ) as the ionic conductor or infiltrated into a porous anode structure, can lead to the reduction or elimination of sulfur poisoning.", "The procedures used by other groups to infiltrate ceria into SOFC anodes usually involve immersing the anodes into a precursor solution, e.g., of cerium nitrate [16,18,22–24] or through a sol–gel route [25].", "After drying and high-temperature treatment, a ceramic film results.", "Recent developments in the aqueous-phase deposition of functional oxides [26] can lead to a greater degree of control over the properties and morphology of films on SOFC anodes.", "Specifically, the surfaces of a commercial SOFC anode were treated with surfactants prior to immersion in an aqueous precursor solution [27].", "By this approach, a nanocrystalline ceria film was formed without further heat treatment.", "The thickness of the film and its morphology and distribution within the microstructure of the porous SOFC anode depended significantly on the type of pretreatment used.", "The present research sought to distinguish sulfur tolerance due to replacing YSZ with ceria from that due to protecting Ni from sulfur exposure.", "Few studies of sulfur poisoning have characterized the microstructural changes associated with the loss of performance [6,19–20 28].", "In the present work the microstructural changes and the degree of sulfur tolerance were related to the presence or absence of the ceria coating, its morphology (which depended on the prior surfactant treatment), and the extent of sulfur exposure.", "Results First we illustrate general characteristics of the performance of the cells in sulfur-containing environments.", "Then SEM and EDXS analyses of the microstructures of the cells, before and after operation, with and without surfactant pretreatments are presented.", "The performance of the cells, grouped by type of anode treatment, is then discussed to show correlations between surfactant treatment, coating characteristics, and cell performance.", "The anode treatments were of four types: Treatment 1: no ceria coating or surfactant treatment Treatment 2: ceria coating with no surfactant treatment (direct-treated) Treatment 3: ceria coating after thiol surfactant treatment Treatment 4: ceria coating after sulfonate surfactant treatment Effects of sulfur exposure on cell performance The initial value of current density for each cell was chosen to give an output voltage of 0.7 V.", "If voltage dropped by more than 10% in a 24 h period, the current density was reduced to raise the voltage back to 0.7 V.", "Common measures of SOFC performance are the change in output voltage over time at a fixed current density, and area specific resistance (ASR, units of Ω·cm2).", "Fig. 1 shows the change in output voltage and ASR in a cell with no ceria coating (treatment 1) running on H2/N2 fuel at 107 mA·cm−2 (8.4% fuel utilization) throughout the 192 h test.", "This cell exhibited sulfur tolerance, i.e., only a gradual loss in power (no worse than that observed in sulfur-free fuel in the first 24 h of operation) throughout the test, though H2S levels progressively increased from 0 and 500 ppm in 24 h intervals.", "Such behavior was observed in many cells operated at current densities below 200 mA·cm−2, regardless of the presence or absence of a ceria coating.", "Figure 1 Output voltage and ASR at low current density, showing sulfur tolerance.", "Yellow shading denotes 24 h periods of H2S exposure in the anode stream at the concentration indicated.", "(Treatment-1 cell (no ceria coating) with no interlayer.)", "Fig. 2 shows the change in output voltage and ASR in a treatment-3 cell operating while H2S levels alternated between 0 and 50 ppm in 24 h periods.", "The current density of 214 mA·cm−2 corresponded to fuel utilization of 16.7%.", "This test showed several hallmarks of sulfur poisoning [4–5 7,10]: a sharp initial drop in voltage on adding 50 ppm H2S to the fuel stream; a slower decrease in voltage on continued operation under constant atmosphere; recovery of most of the lost output voltage on reducing the H2S level to 0 ppm; overall decline in output voltage at constant current density, and a progressive rise in ASR (from 1.3 Ω·cm2 to 4.8 Ω·cm2) over the duration of the test.", "Figure 2 Output voltage and ASR, showing typical effects of partially reversible sulfur poisoning.", "Yellow bands denote periods of H2S exposure in the anode stream at the concentration indicated.", "(Treatment 3 cell, no interlayer.)", "This behavior was typical for many cells operated at current densities above about 200 mA·cm−2 [12], whether ceria-coated or not.", "In general, exposure to H2S led to shorter operating lifetimes and/or lower power (see Fig. 12 below), resulting in lower total lifetime energy output.", "Fig. 3 underscores the significance of current density in the appearance of sulfur poisoning in the present study.", "It shows the change in output voltage and ASR in a treatment-4 cell that exhibited both sulfur tolerance at a current density of 150 mA·cm−2 (24–192 h) and partially reversible sulfur poisoning at 179–200 mA·cm−2 (192–456 h).", "Figure 3 Output voltage and ASR, showing sulfur tolerance at a current density below 200 mA·cm−2 (24–192 h) and partially reversible sulfur poisoning at 200 mA·cm−2 (192–456 h).", "(Treatment-4 cell, no interlayer.)", "Fig. 4 shows the voltage output versus time of a treatment-2 cell that initially showed high sulfur tolerance, with little change in voltage or ASR on exposure to 50 ppm of H2S at high current density (625 mA·cm−2) for 24 h.", "Nevertheless, with each subsequent 24 h increase in H2S level (to 100 and 200 ppm) the current density had to be reduced sharply (to 368 and 129 mA·cm−2, respectively) to maintain the same voltage as at the preceding H2S level.", "(After about 90 h of testing, the rapid failure of the cell resulted from inadequate removal of H2O from the anode atmosphere [12].)", "Figure 4 Output voltage and ASR, showing initial sulfur tolerance at high current density, and early cell failure.", "(Treatment-2 cell with GDC interlayer.)", "Microstructures of as-treated anodes The microstructures of coatings of cells with gadolinia-doped ceria (GDC) interlayers between the anode and electrolyte (see Experimental section for details) were essentially the same as those observed on cells without GDC interlayers.", "All SEM images shown here, except Fig. 9, are of cells without GDC interlayers.", "The as-received anodes (i.e., before reduction of NiO to Ni) (Fig. 5) had a Ni:Ce atomic ratio of 3.47 (22.4 atom % Ce) (Table 1), in excellent agreement with the value of 3.43 computed from their nominal composition.", "(All reported Ni:Ce ratios and cerium concentrations were measured by using energy-dispersive X-ray spectroscopy (EDXS).)", "The NiO particles ranged in size from 0.5 to 1.5 μm and had faceted, polygonal faces (Fig. 5).", "The GDC particles were more rounded; many were sintered agglomerates ca. 3 μm long and ca. 1 μm wide.", "Figure 5 Top views of ceria deposition on NiO/GDC anodes. a) Treatment 1 (no coating). b) Treatment 2 (direct-treated).", "The ellipse indicates a gap in the coating. c) Treatment 3 (thiol-treated). d) Treatment 4 (sulfonate-treated).", "Direct-treated ceria coatings (treatment 2) were mostly uniform and continuous (Fig. 5).", "The presence of a coating can be readily detected in the covering of the polygonal NiO grains, giving them a more rounded appearance.", "The untreated coating exhibited a few cracks at grain boundaries and occasional gaps (indicated by a circle in Fig. 5).", "The Ni:Ce atomic ratio was 2.60 (27.8 atom % Ce) (Table 1).", "Table 1 Summary of typical EDXS analyses of Ce and Ni (Ni + Ce = 100 atom %) from Ni/GDC anodes (without GDC interlayer) in cells before and after testing, by type of pre-treatment.", "Data in the “after testing” columns were taken from the surfaces and cross-sections of the anodes shown in Figures 7 through 10. treatment before testing after testing surface cross- section 1 Ni, atom % 77.6 69.4 69.2 Ce, atom % 22.4 30.6 30.8 Ni:Ce 3.47 2.27 2.25 ∆(Ni atom %)a — −8.2 −8.4 2 Ni, atom % 72.2 64.2 64.4 Ce, atom % 27.8 35.8 35.6 Ni:Ce 2.60 1.79 1.81 ∆(Ni atom %)a — −8.0 −7.8 3 Ni, atom % 66.8 65.3 67.5 Ce, atom % 33.2 34.7 32.5 Ni:Ce 2.01 1.88 2.08 ∆(Ni atom %)a — −1.5 0.7 4 Ni, atom % 76.6 76.8 69.2 Ce, atom % 23.4 23.2 30.8 Ni:Ce 3.27 3.30 2.25 ∆(Ni atom %)a — 0.2 −7.4 aChange in atom % of nickel from start of testing to the end.", "On thiol-treated anodes (treatment 3; Fig. 5) the ceria coating was uniform and continuous.", "Cracks in the coating were occasionally evident at the grain boundaries.", "The Ni:Ce atomic ratio was 2.01 (33.2 atom % Ce) (Table 1).", "On sulfonate-treated anodes (Fig. 5) the appearance of the anode was similar to that of the untreated anode, except that loose ceria clusters were evident.", "The Ni:Ce atomic ratio was 3.27 (23.4 atom % Ce) (Table 1).", "Coating thicknesses were measured on cells with NiO/YSZ anodes that had been coated by using the same procedures as for the nickel-GDC anodes.", "Then cross-sections were prepared by using a focused ion beam unit, and EDXS maps were superimposed on the cross-sectional images (Fig. 6).", "With YSZ replacing the GDC as the ionically conducting phase in the anode, the ceria coating could easily be distinguished.", "All three cross-sections showed ceria coatings enveloping both the NiO and YSZ grains.", "Fig. 6 shows that the coating extended into the porous anode.", "The thicknesses of the coatings were determined from 5–10 locations in the underlying SEM images (not shown).", "Typical thickness values ranged from 60 to 170 nm on the direct-treated anode (Fig. 6), 100–140 nm on the thiol-treated anode (Fig. 6), and 50–110 nm on the sulfonate-treated anode (Fig. 6).", "Coating thicknesses typically varied in the order: thiol (treatment 3) > direct (treatment 2) > sulfonate (treatment 4).", "The ceria contents of these samples, as determined from overall EDXS analysis of the SEM images, decreased in the same order (Table 1, Ce atom % before testing).", "Figure 6 FIB cross-sections halfway through ceria-coated NiO/YSZ anodes, with superimposed EDXS maps (Ni: green; Zr: blue; Ce: yellow). a) Direct deposition (treatment 2). b) Deposition after thiol treatment (treatment 3). c) Deposition after sulfonate treatment (treatment 4).", "(Pink regions are the protective Pt layer applied as part of the FIB sectioning technique.)", "Microstructural analysis of anodes after operation As-received cells (treatment 1): Fig. 7 shows the post-operation cross-sectional SEM images of the anode of an as-received cell (i.e., no ceria coating).", "The cell was tested at an average current of 71 mA·cm−2 for 98 h with a total H2S exposure of 28.8 cm3.", "Even during this short test at low current density, some of the Ni particles had coarsened to over 2 μm in size (vs 0.5 to 1.5 μm before testing, Fig. 5).", "At the top of the anode, coarsened Ni particles were spread on the surface.", "Both Ni particles and GDC particles were rounded without facets.", "The Ni:Ce atomic ratio was 2.27 at the surface and 2.25 at the cross-section, compared to 3.47 as received (Table 1).", "That is, Ni was depleted from the anode during operation, but had not preferentially segregated to the surface.", "Figure 7 Cross-sectional view of an untreated Ni/GDC anode (treatment 1) after operation. a) SEM image; b) EDXS mapping of Ni (green) and Ce (yellow).", "Direct-coated cells (treatment 2): Fig. 8 shows the anode of a direct-treated cell that gave an average current density of 135 mA·cm−2 for 109 h, with a total H2S exposure of 28.9 cm3.", "The testing conditions were comparable with the cell shown in Fig. 7, but at nearly twice the current.", "The Ni:Ce atomic ratio was 1.79 at the surface, and 1.81 over the entire cross-section, compared to Ni:Ce = 2.60 at the surface of the coated anode before operation, i.e., depletion of Ni had occurred during operation, but Ni had not preferentially segregated to the surface.", "Figure 8 Cross-sectional view of a direct-treated anode (treatment 2) after cell operation. a) SEM image; b) EDXS mapping of Ni (green) and Ce (yellow).", "Thiol-treated cells (treatment 3): Fig. 9 shows the anode of the thiol-treated cell of Fig. 2 after operation (average current density of 218 mA·cm−2 for 305 h of actual operation, with a total H2S exposure of 36 cm3).", "This test lasted nearly three times as long as that of the direct-treated cell (Fig. 8).", "After operation, the remaining ceria film and film fragments could be observed at the anode surface and near the electrolyte (Fig. 9).", "A few coarsened Ni particles over 2 μm in diameter, round with smooth surfaces, protruded from the anode surface.", "Pieces of the ceria film or of GDC particle fragments were observed on the coarsened Ni particles.", "The measured Ni:Ce ratio was 1.88 at the anode surface, and 2.08 over the cross-section (compared with 2.01 at the surface before operation).", "That is, a slight loss of Ni from the surface had occurred.", "Figure 9 Cross-sectional views of the thiol-treated anode (treatment 3) of the cell shown in Fig. 2 after operation. a) Whole anode thickness; b) EDXS mapping of Ni (green) and Ce (yellow); c) and d) higher magnification, c) near the anode surface and d) near the electrolyte (electrolyte is visible at bottom).", "Images c) and d) show that the ceria coating persisted throughout the anode.", "(Arrows in d point to coating edges or cracks).", "Sulfonate-treated cells (treatment 4): Fig. 10 shows the anode of the sulfonate-treated cell of Fig. 3 after testing (average current density of 187 mA·cm−2 for 456 h, with a total H2S exposure of 367 cm3).", "This was the longest test and the highest cumulative H2S exposure of the cells shown in Figures 1–4 and 7–10.", "Nickel and ceria phases were sintered into a porous two-phase network, with no signs of a ceria coating remaining.", "The measured Ni:Ce atomic ratio for the cross-section was 2.25, compared with 3.27 on the surface before operation, suggesting that nickel depletion from the interior had occurred during operation.", "Figure 10 Cross-sectional view of a sulfonate-treated anode (treatment 4) after operation. a) SEM image; b) EDXS mapping of Ni (green) and Ce (yellow).", "The loss of Ni from the anodes was especially noticeable for uncoated cells.", "Among the 17 anodes whose Ni distributions were analyzed after testing, on average, the trend for significance of this effect was: treatment 1 > treatment 4 ≈ treatment 2 > treatment 3.", "That is, the thicker the ceria coating, the less severe was loss of Ni from the anode.", "Overall cell performance Because the test protocol (see Experimental section) subjected the cells to a wide range of current densities and H2S exposures of various concentrations and durations (compare, e.g., Figures 1–4), and because of the different pre-treatments to which the cells were subjected, as well as performance variations between nominally identical cells, the cells exhibited significant variation in their operating lifetimes and output.", "As fuel cells are essentially energy-conversion devices, one useful metric for assessing the relative performance of devices that differed not only in their anode structures, but also in the details of their operating history, is total electrical energy output over the life of the device.", "Fig. 11 shows the average total energy output of the cells (with and without GDC interlayers), grouped by anode treatment, in tests entailing H2S exposure.", "On average, the direct-treated and thiol-treated cells provided 103% and 78.5% more energy over their lifetimes than did the untreated cells, whereas the sulfonate-treated cells provided 31% less energy than the untreated cells.", "Figure 11 Average lifetime energy output of SOFCs (with and without GDC interlayers) tested in sulfur-containing fuel streams, grouped by treatment: 1, no coating; 2, direct ceria coating; 3, ceria coating after thiol treatment; 4, ceria coating after sulfonate treatment.", "The numeral above each column is the number of cells tested for each type of treatment.", "Plotting the average power over the lifetime of individual cells versus total H2S exposure for the four types of treatment (Fig. 12, which includes all of the cells averaged in Fig. 11, plus cells that underwent no H2S exposure) gives another perspective on the effectiveness of the ceria coatings at improving sulfur tolerance.", "For cells with the same treatment, the average power mostly decreased with increasing cumulative sulfur exposure over the cell lifetime, but only ceria-coated cells (treatments 2, 3, and 4) survived total H2S exposure greater than 120 cm3.", "Fig. 12 also indicates that for cells that experienced no H2S exposure, all the ceria-coated cells exhibited higher average power than the uncoated cells (treatment 1).", "This suggests that the ceria coating, regardless of the details of the pre-treatment, improved the average power output of the cells over their lifetimes.", "Figure 12 Average power over cell lifetime, grouped by anode treatment and anode type, ranked by cumulative H2S exposure within each group.", "Numbers at the top of each column indicate the cumulative H2S exposure over the lifetime of each cell.", "Blue columns: cells with GDC interlayers between anode and electrolyte.", "Red columns: cells without GDC interlayers.", "Discussion The microstructures of the anodes changed greatly during operation and depended strongly on the testing conditions.", "The most notable changes occurred in the nickel phase: coarsening (in almost all cases), and nickel depletion from the interior in most anodes.", "The effects of the coatings and of the surfactant treatments on these phenomena are discussed below.", "Dependence of coating characteristics on surfactant treatments Whatever effects the organic surfactants had on the cell performance could have only been exerted during the deposition of the ceria coatings.", "Before cell operation, during the high-temperature reduction of NiO to Ni (see Experimental section), the surfactants were undoubtedly burnt out, as similar surfactant layers have been shown to pyrolyze below 400 °C, even in low-oxygen atmospheres [29].", "During deposition, the solution parameters (concentration, temperature, and pH) can be expected mainly to dictate the particle size and ultimate crystalline form of the coating [30].", "The effects of the surfactant layer will be seen primarily in the extent to which it promoted the attachment of the solid particles from the deposition medium and affected their distribution on the substrate (in this case, a NiO–GDC composite).", "In previous studies of oxide film deposition on surfactant-treated surfaces, sulfonate surfaces strongly favored the formation of continuous films of ZrO2, TiO2, and SnO2 [26].", "This outcome is attributed to the high negative surface charge density of well-packed sulfonate surfaces under the acidic conditions at which these oxides precipitate from solution [31].", "When the same treatments that we described here were used prior to applying ceria coatings to a different SOFC anode design than that used in the current work [27], the sulfonate surface gave the thickest and most continuous coatings.", "In the present study, the fact that the sulfonate treatment gave the thinnest and least uniform ceria coatings can be attributed to the nature of the deposited surfactant layer.", "X-ray photoelectron spectroscopy (XPS) of the sulfonate-treated anodes (before ceria deposition) showed carbon and sulfur signals much higher than expected [32] from, e.g., a well-packed surfactant monolayer, and many times higher than the signals detected in the sulfonate-treated anodes of [27].", "This indicates that the sulfonate treatment on the present anodes left large oligomers and cross-linked clusters of surfactant, which could have obscured or neutralized most of the sulfonate functionality and led to the thinner, less uniform ceria coatings.", "Conversely, XPS measurements of the thiol-treated anodes before ceria deposition showed that most of the thiol functionality had oxidized to sulfonate.", "So it appears in the present work that the thiol surfactant provided a surface more like a well-packed sulfonate layer than did the sulfonate treatment (Figures 5c vs 5d; Figures 6b vs 6c), resulting in thicker and more uniform ceria coatings from the thiol treatment than from the sulfonate treatment.", "Relation of cell performance to coating characteristics and surfactant treatments The effects of the surfactant treatments on the coatings are reflected in the sulfur tolerance of the variously treated anodes (Fig. 11 and Fig. 12).", "In light of the current thinking that sulfur blocks catalytic sites for the anode reaction on the nickel, the ceria coating may act to impede the sulfur adsorption on the nickel while still allowing the anode reaction to proceed.", "The current results then suggest that a continuous coating (direct- or thiol-treated), but not necessarily the thickest (thiol-treated) provides best sulfur tolerance to the anode.", "Aspects of the sulfonate treatment, particularly the oxone oxidation step, may have adversely affected the anode surface chemistry.", "(As explained in the Experimental section, we observed chemical damage to the cathode if the oxone solution contacted it, and subsequently took steps to prevent such contact before testing began.)", "Nickel coarsening Coarsening of nickel is often associated with performance degradation in cermet SOFC anodes [3,16,33–34].", "One significant effect of the ceria coating in the current work was to hinder nickel coarsening.", "For example, compare the significantly coarsened nickel in Fig. 7 (an untreated cell) to the nickel in Fig. 8 (an direct-treated cell), tested for a similar time but at twice the current and power.", "Similarly, compare Fig. 7 to Fig. 9 and Fig. 10 (thiol- and sulfonate-treated cells), which showed similar coarsening though the coated cells experienced many times longer and more intensive operation.", "Coarsening of the metallic phase reduces the density of three-phase boundaries between pore, electronic conductor, and ionic conductor, which are essential to cell operation [35].", "Coarsening of Ni also leads to less interconnection of metal particles and therefore to a decrease of the electrical conductivity of the anode.", "This would be expected to result in loss of power over time, e.g., increased ASR.", "The ceria coatings could not suppress nickel coarsening indefinitely.", "The coatings were readily observed after early stages of cell operation, but in the anodes of long-lived cells the ceria coating was visible mainly as small fragments on coarsened nickel particles.", "Most of the coating had presumably sintered into, and was indistinguishable from, the GDC phase of the anode.", "This suggests that eventually the ability of the coating to hinder coarsening broke down, allowing coarsening to proceed until the cell failed.", "Nickel depletion Lussier et al. [8] reported Ni depletion from Ni/YSZ and Ni/GDC anodes during operation in sulfur-containing atmospheres.", "Likewise in the present work, by comparing the anode composition before and after cell operation, loss of nickel from the anode was detected for most cells, especially uncoated cells and cells running at high current for long times [32,36].", "This suggests that the ceria coatings hindered Ni depletion.", "The mechanism of nickel depletion is believed to involve the formation of low-melting, volatile Ni(OH)2 in the presence of the H2O formed at the anode [37].", "A ceria shell around the metal network may act as a physical barrier to impede Ni(OH)2 formation or evaporation, with the most continuous coatings being most effective.", "Conclusion Overall, this work established that nanocrystalline ceria coatings could be deposited throughout porous cermet anodes of SOFCs 6 μm thick by using an aqueous infiltration technique at 50 °C in 48 h without subsequent heat treatment.", "The morphology of the coatings – specifically, their thickness and their continuity – could be affected through surfactant pretreatments.", "Lastly, continuous uniform coatings 60–170 nm thick, as deposited directly on the anodes without prior surfactant treatment, or 100–140 nm thick as deposited on thiol-treated anodes, significantly improveed the sulfur tolerance in the tested cells.", "The improvements in sulfur tolerance in ceria-coated anodes were attributed to the ability of the coatings to suppress Ni coarsening and depletion in the anode, and this effect was most pronounced in the thiol-treated and the direct-treated cells.", "The protective effect of the ceria coating appeared to diminish in cells where the coating had not remained physically intact and continuous.", "Experimental The cells used in this study were electrolyte-supported, circular “button” cells, 3.8 cm in diameter.", "The electrolyte was Y0.03Zr0.97O2−δ, 100 μm thick.", "The anode, 6 μm thick, consisted of 60 wt % NiO and 40 wt % Gd0.1Ce0.9O2−δ (gadolinia-doped ceria, GDC).", "The NiO was reduced to Ni during the initial heat-up of the cell under a flowing H2/N2 stream before cell operation began.", "Some anodes (the cell of Fig. 4, cells included in the averages in Fig. 11, and cells represented by blue columns in Fig. 12) in addition contained a 2 μm-thick, porous GDC interlayer between anode and electrolyte.", "This interlayer had no discernible effect on the characteristics of the ceria coatings, either before or after testing, which are the focus of the current work; the conclusions presented here apply equally to both of these types of anodes.", "The cathode, 12 μm thick, was composed of 50 wt % Y0.08Zr0.92O2-δ and 50 wt % lanthanum strontium manganite with La:Sr ratio of 0.85:0.15.", "The area of each electrode was 2.8 cm2.", "Surfactant treatment and ceria deposition All cells were first cleaned with ethanol and dried in flowing argon.", "For the thiol treatment, the cleaned substrates were immersed in 1-dodecanethiol (CH3C11H22SH) for 5 h at room temperature in air, then washed in flowing ethanol for 2 min and in deionized water for 2 min.", "For the sulfonate treatment, the cleaned cells were immersed in 1 vol % 1-bromo-11-(trichlorosilyl)undecane (Cl3SiC11H22Br) in bicyclohexyl (C12H22) for 5 h at room temperature in air.", "The trichlorosilyl groups hydrolyze and undergo condensation reactions with oxide and hydroxide groups on the electrode surfaces, and with each other.", "The intended result is a siloxy-anchored, bromine-terminated, cross-linked organic monolayer on the pore walls of the electrode.", "Then the specimens were refluxed with 7% potassium thioacetate in ethanol at 80 °C for 16 h to replace the –Br end groups with thioacetate (-SCOCH3).", "Lastly, the thioacetate was converted to sulfonate (-SO3H) by exposing the anode to saturated oxone (2KHSO5·KHSO4·K2SO4) aqueous solution for 2.5 h at room temperature [31].", "During this step, instead of immersing the cell into the oxone solution, a cotton pad saturated with oxone was used to cover only the anode side of the cell.", "This technique provides enough oxone to oxidize the thioacetate group to sulfonate, while preventing damage to the cathode by reaction with the oxone.", "Prior to ceria deposition, the surfactant depositions were monitored with X-ray photoelectron spectroscopy (XPS, PHI Model 5600 MultiTechnique System), with particular attention to the presence of the characteristic functional groups and to the progress of the in situ transformations entailed by the sulfonate treatment.", "To deposit the ceria coating, the cells (with or without surfactant pre-treatment) were immersed in an aqueous solution of 0.01 M cerium acetate and 0.005 M potassium chlorate [38] at 50 °C for 48 h.", "After the deposition, the cells were rinsed with deionized water then ethanol and dried with argon.", "Cell operation Current collectors, consisting of a Pt wire (Alfa Aesar, 0.30 mm dia., 99.9% metals basis) spot-welded to Pt mesh (Alfa Aesar, 52 mesh, woven from 0.1 mm-diameter wire, 99.9% metals basis), were bonded to both electrodes with Pt-based ink (Heraeus).", "The cell was then sealed to the end of a 3.2 cm-diameter stabilized zirconia tube (by using a silicate-based paste fired at 1050 °C for 1 h) with the anode facing an alumina gas feed tube inside the zirconia tube.", "This assembly was then put into a vertical tube furnace for cell operation.", "Cell operation was conducted at 900 °C.", "The cathode side of the cell was exposed to the air atmosphere of the furnace.", "Fuel of 25 sccm H2 and 25 sccm N2, humidified to 3% water vapor by passing through a water bubbler at room temperature, was fed to the anode through the alumina tube.", "For each tested cell, open circuit voltage (OCV) was checked at the start of operation and every 24 h thereafter to be between 1.0 and 1.1 V, and testing was ended if the OCV was below 1.0 V.", "Cells were operated galvanostatically (by using an Autolab electrochemical analyzer or an Amrel electronic load with a power supply) at a current that produced a cell voltage of 0.7 V.", "If the cell voltage dropped more than 5% in 24 h, the current was reduced until the voltage reached 0.7 V.", "If the cell voltage dropped less than 5% in the first 24 h, H2S was introduced to the fuel stream at 50 ppm for an additional 24 h.", "If the cell voltage dropped by less than 5% during this period, the level of H2S was raised to 100 ppm, 200 ppm, 300 ppm, 400 ppm, or 500 ppm in successive 24 h periods.", "If the voltage dropped by more than 5% during any of these stages, the cell was run in the original sulfur-free gas flow for 24 h.", "Testing was ended if the voltage dropped to 0.4 V or if the current density had dropped to <50 mA/cm2 after a long decline in performance.", "After operation, the cells were cooled in flowing humidified H2/N2 to near room temperature.", "The current collectors were carefully peeled from the electrodes before analysis.", "Cell characterization Scanning electron microscope (SEM) images of the anodes were taken (FEI xT Nova Nanolab) at 5 kV accelerating voltage.", "Energy-dispersive X-ray spectroscopy (EDXS) mapping at beam energy of 15 keV, combined with SEM images, was used to resolve the phases of anode particles qualitatively and to investigate the microstructure changes.", "The chemical compositions of the anode were analyzed (QUANTAX Esprit 1.8 software) on EDXS maps taken over an area of 190 μm2 or greater.", "Cross-sectional images through the coated anodes were obtained by using the focused ion beam unit of the Nova Nanolab." ]

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[ "High performance anode-supported tubular solid oxide fuel cells fabricated by a novel slurry-casting method High performance anode-supported tubular solid oxide fuel cells fabricated by a novel slurry-casting method DuanNan-Qi1YanDong1ChiBo1PuJiana1JianLi1 1Center for Fuel Cell Innovation, State Key Laboratory of Coal Combustion, School of Materials Science and Engineering, Huazhong University of Science and Technology, Wuhan, Hubei 430074, China apujian@hust.edu.cn 8174 Tubular solid oxide fuel cells were fabricated and evaluated for their microstructure and electrochemical performance.", "The tubular substrate was prepared by casting NiO-Y2O3 stabilized ZrO2 (YSZ) slurry on the inner wall of a plastic mold (tube).", "The wall thickness and uniformity were controlled by slurry viscosity and rotation speed of the tube.", "The cells consisted of Ni-YSZ functional anode, YSZ electrolyte and (La0.8Sr0.2)0.95MnO3-δ (LSM)-YSZ cathode prepared in sequence on the substrate by dip-coating and sintering.", "Their dimension was 50 mm in length, 0.8 mm in thickness and 10.5 mm in outside diameter.", "The peak power density of the cell at temperatures between 650 and 850°C was in the range from 85 to 522 mW cm−2 and was greatly enhanced to the range from 308 to 1220 mW cm−2 by impregnating PdO into LSM-YSZ cathode.", "During a cell testing at 0.7 A cm−2 and 750°C for 282 h, the impregnated PdO particles grew by coalescence, which increased the cathode polarization resistance and so that decreased the cell performance.", "According to the degradation tendency, the cell performance will be stabilized in a longer run.", "A solid oxide fuel cell (SOFC), consisting of porous anode and cathode separated by a dense electrolyte, is an electrochemical device, which efficiently and environment friendly converts the chemical energy of fossil and hydrocarbon fuels into electricity and heat without involving combustion and mechanical motion.", "The operating temperature of SOFCs was near 1000°C, and has been lowered to the intermediate-temperature range between 650 and 800°C for the benefits in materials selection, performance durability and manufacturing cost by taking the anode-supported and thin electrolyte cell configuration.", "It is also realized that the electrocatalytic activity of conventional cathode materials, such as Sr-doped LaMnO3, is lower at intermediate temperatures and needs to be improved for achieving high cell performance.", "The most popular types of cell design for SOFCs are tubular and planar.", "The tubular cell has advantages in sealing, cell-to-cell connection1, thermal cycling and start-up because of its symmetric geometry2.", "Many techniques for tubular cells fabrication have been reported in recent years, such as extrusion34567, iso-pressing8 slip casting9 and dip-coating1011.", "In the present study, a novel “slurry-casting” method was developed for preparing the tubular anode-support, on which functional anode and electrolyte were dip-coated in sequence before co-firing.", "This method is easy to operate, cost effective and applicable to both laboratory and industry scale fabrication of tubular cells.", "In this paper, the microstructure and performance of such prepared tubular cells are reported.", "The cells consisted of conventional Ni-Y2O3 stabilized ZrO2 (Ni-YSZ) cermet anode, YSZ electrolyte and (La0.8Sr0.2)0.95MnO3-δ (LSM)-YSZ cathode; and their performance was greatly enhanced by Pd modification of the cathode.", "Results The sintered cell was 50 mm in length, ~0.8 mm in wall thickness and ~10.5 mm in outside diameter (Supplementary Fig.", "S1).", "After reduction during the cell test, the porosity of the anode-support was about 38%; and the functional anode, electrolyte and cathode were well adhered to each other with a uniform thickness of approximately 25, 15 and 15 μm (Supplementary Fig.", "S2), respectively.", "In the Pd-modified LSM-YSZ cathode (Pd+LSM−YSZ), nano-sized PdO particles (20–50 nm) were uniformly distributed on the LSM-YSZ scaffold by solution impregnation.", "Fig. 1 demonstrates the microstructure of the as-prepared LSM-YSZ (Fig. 1a) and Pd+LSM−YSZ (Fig. 1b) cathodes and the tested Pd+LSM−YSZ (Fig. 1c) cathode.", "Fig. 2 shows the I-V-P curves of prepared cells (active area 3 cm2) at temperatures between 650 and 850°C with H2 as the fuel and air as the oxidant.", "Their open circuit voltage was higher than 1.1 V, suggesting that the cells were properly sealed and the electrolyte was gas tight without fuel crossover.", "Without adding PdO particles into LSM-YSZ cathode, the peak power density varied from 85 to 522 mW cm−2 (Fig. 2a) at temperatures from 650 to 850°C; whereas it was increased more than twice to the range from 308 to 1220 mW cm−2 (Fig. 2b) at the same temperatures by impregnating PdO particles into the cathode.", "In order to evaluate the long-term performance of the cell with Pd+LSM-YSZ cathode, it was tested at 0.7 A cm−2 and 750°C for 282 h, as shown in Fig. 3.", "After the initial voltage increasing from 0.753 to 0.782 V, possibly due to electrochemical activation of the LSM-YSZ1213, the voltage decreased almost linearly at a rate of 0.39 mV h−1 for around 170 h before the degradation rate changed to a lower value of 0.17 mV h−1.", "Discussion As shown in Fig. 2, the cell performance at open circuit voltage and temperatures between 650 and 850°C was greatly enhanced by impregnating PdO particles into the LSM-YSZ cathode.", "This phenomenon was intensively studied141516 in our group.", "It was found that cathode polarization resistance was greatly reduced, especially for the low-frequency one, due to the redox reaction between Pd and PdO that facilitated the low-frequency electrode processes of oxygen adsorption and dissociation in the cathode.", "It was also observed that the performance of the cell with Pd+LSM−YSZ cathode decreased at a gradually slowed rate over time at 0.7 A cm−2 and 750°C (Fig. 3).", "Since the Ni-YSZ anode, electrolyte and LSM-YSZ scaffold are stable under the testing conditions1718, as demonstrated by Supplementary Fig.", "S3 for the durability of the cell with the LSM-YSZ cathode, the performance degradation is expected to be related to the microstructure change of the impregnated particles1920.", "The original nano-sized PdO particles coalesced into larger particles on the surface of the scaffold during the test at 750°C, as shown in Fig. 1c, which decreased the surface area of the impregnated particles and triple phase boundary, and in turn the cell performance.", "Fig. 4 shows the electrochemical impedance spectra of the cell measured at 0 and 90 h during the durability test.", "The ohmic resistance remained almost constant at around 0.22 Ω cm−2, but the polarization resistance increased from 0.81 to 2.27 Ω cm−2.", "The electrochemical performance of the Ni-YSZ anode and LSM-YSZ cathode was proved to be stable (Fig.", "S3); therefore it is reasonable to consider that the polarization resistance increase was related to the infiltrated PdO particles.", "By data fitting the impedance spectra according to the equivalent circuit shown in Fig. 4, the high- and low-frequency polarization resistances were determined.", "The low-frequency polarization resistance was increased by almost 5 times from 0.24 to 1.20 Ω cm2 and the high-frequency one was increased by less than 2 times from 0.57 to 1.07 Ω cm2.", "This result provides another evidence for that the cell performance was compromised by the increase of both the low- and high-frequency polarization resistances, particularly the low-frequency one, due to the growth of the impregnated particles.", "As the growth rate of the impregnated particles slows down, the cell performance will gradually approach to a stable level (Fig. 3).", "To avoid such cell performance degradation, the microstructure of the Pd+LSM−YSZ cathode should be stabilized by adding alloying elements into PdO particles20.", "Methods Fuel cell fabrication The tubular substrate with one closed end was made from the composite powder consisting of 57 wt% NiO and 43 wt% YSZ by a slurry-casting method.", "The slurry was prepared by ball milling for 24 h with xylene and ethanol as the solvents, fish oil as the dispersant, corn starch as the pore former, polyvinyl butyral as the binder and butyl benzyl phthalate as the plasticizer.", "The ball-milled homogeneous slurry was poured into a tubular plastic mold and degassed, while it was rotated at a speed of 2000 r min−1 for 2 min in a centrifugal machine.", "Slurry viscosity was carefully adjusted to between 16000 and 20000 mPa s, so that it wetted the plastic mold perfectly, forming a layer of slurry that covered the inner wall of the mold after extra slurry was poured out in a container for reuse.", "The slurry hanging on the wall of the mold was gradually dried and detached from the mold automatically due to shrinkage, while the mold was rotated vertically on a rotating plate at a constant angular velocity.", "The thickness and uniformity of the substrate tube was controlled by slurry viscosity and rotating speed.", "Finally, a crack-free green tubular NiO-YSZ substrate was obtained with a uniform wall thickness and smooth surfaces (Supplementary Fig.", "S1).", "The dried substrate was heated slowly for debinding and pre-sintered at 1000°C.", "For fabrication of the functional anode and electrolyte, slurries containing 30 wt% NiO-YSZ (same composition as above) and 40 wt% YSZ, respectively, were prepared with terpilenol or ethyl alcohol as the solvent and ethyecellulose or polyvinyl butyral as the binder, and dip-coated in sequence on the outer surface of the pre-sintered NiO-YSZ substrate (Supplementary Fig.", "S1), prior to co-firing at 1390°C for 3.5 h.", "Composite LSM-YSZ cathode, containing 50 wt% LSM and 50 wt% YSZ, was applied on the top of the YSZ electrolyte also by dip-coating using a slurry prepared in a similar way to the above, and fired at 1150°C for 2 h to obtain a tubular anode-supported cell.", "To enhance the cell performance, PdO was introduced into the LSM-YSZ composite cathode by impregnation of PdCl2 solution with a Pd concentration of about 0.5 mol L−1 and subsequent calcination at 700°C in air for 1 h.", "Ammonium hydroxide was added into the solution to adjust pH value to 8.", "The loading of the impregnated PdO in the cathode was about 1.2 mg cm−2 after repeating the process for 5 times.", "Fuel cell test The cell performance was evaluated by using an in-house developed testing setup (Supplementary Fig.", "S4).", "The cell was sealed by using a ceramic sealant.", "Ni foam was rolled up and squeezed into the tubular cell as the anode current collector.", "Pt paste painted on the cathode and Ag wire were used as the cathode current collector.", "Pure H2 was fed to the anode at a rate of 200 ml min−1; and ambient air was blown into the furnace at a rate of 300 ml min−1.", "Characterizations Electrochemical measurement was carried out by using a Solartron 1260 frequency response analyzer (Solartron Analytical Ltd.) in a frequency range from 1000 kHz to 0.1 Hz with a signal amplitude of 10 mV at open circuit.", "The long term durability test was performed by using a DC power source (IT-6720, iTech).", "The microstructure of the cell was examined by a scanning electron microscope (SEM, Sirion 200 and Quanta 200, Holland FEI Company)." ]

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[ "Surface engineering of nanoporous substrate for solid oxide fuel cells with atomic layer-deposited electrolyte Surface engineering of nanoporous substrate for solid oxide fuel cells with atomic layer-deposited electrolyte JiSanghoon1TanveerWaqas Hassan2YuWonjong2KangSungmin3ChoGu Young2KimSung Han4AnJihwan5§ChaSuk Won12¶ MottaNunzio Associate Editor 1Graduate School of Convergence Science and Technology, Seoul National University, Iui-dong, Yeongtong-gu, Suwon 443-270, South Korea 2Department of Mechanical Engineering, Seoul National University, Gwanak-ro, Gwanak-gu, Seoul 151-742, South Korea 3Department of Mechanical Engineering, Korea Advanced Institute of Science and Technology, Daehak-ro, Yuseong- gu, Daejeon 305-701, South Korea 4Corporate R&D Institute, Samsung Electro Mechanics, Maeyoung-ro, Yeongtong-gu, Suwon 443-743, South Korea 5Manufacturing Systems and Design Engineering Programme, Seoul National University of Science and Technology, Gongneung-ro, Nowon-gu, Seoul 139-743, South Korea §Tel.: +82-2-970-7276; fax: +82-2-974-5388 ¶Tel.: +82-2-880-8050; fax: +82-2-880-1696 10.3762/bjnano.6.184 Summary Solid oxide fuel cells with atomic layer-deposited thin film electrolytes supported on anodic aluminum oxide (AAO) are electrochemically characterized with varying thickness of bottom electrode catalyst (BEC); BECs which are 0.5 and 4 times thicker than the size of AAO pores are tested.", "The thicker BEC ensures far more active mass transport on the BEC side and resultantly the thicker BEC cell generates ≈11 times higher peak power density than the thinner BEC cell at 500 °C. anodic aluminum oxide atomic layer deposition bottom electrode catalyst mass transport solid oxide fuel cell Introduction Recently solid oxide fuel cells with thin film ceramic electrolytes, called thin film solid oxide fuel cells (TF-SOFCs), have drawn attention as efficient power-generation devices delivering a satisfactory power density (above 1 W/cm2) even below 600 °C stemming from the low ohmic resistance of thin film electrolytes [1–2].", "However, their small active cell area resulted in insufficient output power, which required research on ways to enlarge the active cell area.", "In this regard, the use of scalable and porous substrates is one of the ways, among which anodic aluminum oxide (AAO) membranes are considered as prospective substrates due to their compatible thermal expansion properties with ceramic electrolytes, low corrosiveness, and easy manufacturing [3].", "Furthermore, not containing any metallic particles, AAO substrates are advantageous on the thermo-mechanical durability compared to conventional substrate such as porous cermets [4].", "Thin film electrolytes supported on porous substrates are generally vulnerable for pinhole issues causing gas permeation and electrode diffusion due to the rough surface of porous substrates [5].", "This drawback necessitates conformal and dense thin film electrolytes, and can appreciably be relieved with an aid of atomic layer deposition (ALD) technique that is governed by binary reaction sequence chemistry in vacuum state [6].", "Still, ALD-prepared electrolytes have rarely been utilized in porous substrate-supported SOFCs in spite of their superior characteristics; this was because the expectation that they could diminish the triple phase boundary (TPB), the meeting site between the electrolyte, the electrode, and the fuel, length and disturb the inflow of fuel at bottom electrode catalyst (BEC) side by excessive infiltration into the fuel channel [7–8].", "Study on the thickness of the BEC, which could mitigate the infiltration issue, is therefore crucial in realizing the reliable TF-SOFC structure based on porous substrates such as AAO membranes.", "In this study, the microstructural design of BECs in AAO supporting TF-SOFCs with ALD thin film electrolytes is discussed in terms of their impacts on the electrochemical performance of the cells.", "AAOs with 80 nm-sized pores are used as substrates, and the thicknesses of BECs are smaller or larger than the size of AAO pores.", "Although the 320 nm-thick BEC cell has slightly worse reaction kinetics, compared to the 40 nm-thick BEC cell, its peak power density is approximately 11 times higher due to far more active mass transport on the BEC side.", "Results and Discussion Highly dense ALD thin film electrolyte Thin films fabricated via low-temperature vacuum deposition techniques typically have lower packing density than powder-processed thin films due to the presence of high density of grain-boundaries inside the thin films [9–10].", "The density (≈5.8 g/cm3) of yttria-stabilized zirconia (YSZ) thin films fabricated via ALD technique is, in like manner, lower than that (≈6.1 g/cm3) of powder-processed YSZ [11]; nevertheless, the applied ALD process produced highly densified YSZ thin films compared to high-vacuum sputtering producing YSZ thin films with a density of ≈5.3 g/cm3 (i.e., sputtering has been widely used for fabricating electrolytes for TF-SOFCs).", "Cell performance and microstructural analysis Because the AAO substrate used as a supporter for membrane electrode assembly is non-conductive and catalytically inactive, BEC needs to be coated on the AAO substrate prior to the electrolyte deposition for the anode side current collection and catalytic reaction.", "We considered the reaction kinetics at the BEC–electrolyte interface and fuel transport through AAO pores as the main design parameters in BEC coating.", "To investigate the effects of BEC thickness on the electrochemical performance, polarization curves were plotted for 40, 320, and 480 nm-thick BEC cells having 210 nm-thick ALD YSZ electrolyte and 60 nm-thick top electrode catalyst (used as cathode), referred to the Cell-A, Cell-B, and Cell-C (Fig. 1).", "Three kinds of cells generates high open circuit voltages (OCVs) of ≈1.17 V implying the high integrity of conformal and dense YSZ electrolytes, which is quite contiguous to the theoretical OCV value of 1.18 V under the operating conditions [12].", "However, the overall voltage drop of the Cell-A with increasing current density is much bigger than that of the Cell-B, which results in a ≈11 times lower peak power density (8.8 mW/cm2) compared to that of Cell-B (93.1 mW/cm2).", "In particular, as shown in Fig. 1, the voltage drop of the Cell-A at high current densities (near ≈19 mA/cm2) is considerably sharp, which means that the Cell-A suffers from serious concentration loss compared to the Cell-B [13].", "Owing to the prominent voltage drop at current densities above 100 mA/cm2, the peak power density (65.3 mW/cm2) of the Cell-C was somewhat smaller than that of the Cell-B (Fig. 1).", "This performance reduction may be due to the impoverished mass transport and shortened TPB length caused by excessively thick BEC, which is parallel to previous research discussing the effects of the thickness and microstructure of BECs [14].", "Figure 1 I–V and power density curves, measured at 500 °C, for 80 nm pore AAO supporting (A) 40, (B) 320 and 480 nm-thick bottom electrode catalyst (BEC, sputtered Pt anode deposited under high-vacuum) solid oxide fuel cells, referred to the Cell-A, Cell-B and Cell-C, having 210 nm-thick atomic layer-deposited (ALD) yttria-stabilized zirconia (YSZ) electrolyte and 60 nm-thick top electrode catalyst (sputtered porous Pt cathode).", "To examine the diffusion characteristics of ALD YSZ on the BEC side, 50 nm-thick ALD YSZ was deposited on BECs with different thicknesses, whose cross-sectional microstructure was investigated by focused ion beam and field emission scanning electron microscopy (FIB/FE-SEM) imaging: the BECs were 40 nm and 320 nm in thickness.", "In case of the thinner BEC, a significant amount of ALD YSZ certainly infiltrates into the interior of the BEC as well as into AAO pores (the left image of Fig. 2), which may have negative impacts on fuel supply through AAO pores.", "In case of the thicker BEC, on the other hand, most of the conformal YSZ is deposited on the top surface of the BEC, as shown in the right image of Fig. 2.", "The thicker BEC could remarkably alleviate the infiltration of ALD YSZ into the interior of AAO pores.", "This pronounced difference in infiltration aspect of ALD YSZ should be closely linked to growth characteristics of sputtered films [12].", "The thickness increase of physical vapor-deposited (PVD) films deposited on AAO pores expands their column-width and reduces the size of pinholes (or voids) existing in the sputtered films.", "We thus think that the merging of columnar grains of BEC according to the thickness increase lowers the infiltration degree of ALD YSZ into the BEC and AAO pores.", "This consideration is parallel to the interpretation from the I–V analysis result of Fig. 1 discussed in the previous section.", "Meanwhile, the existence of a few nanometer-sized pinholes formed throughout the thicker BEC, which could provide the physical space to diffuse H2 gas supplied to the anode side, implies the possibility of TPB formation on the BEC side (Fig. 2).", "The transmission electron microscopy and energy-dispersive X-ray (TEM-EDX) quantitative analysis result in the middle of the thicker BEC (at dotted asterisk) verified the constituent elements of Pt (78.9%), Zr (6.9%), Y (0.5%), and O (13.7%), meaning that such pinholes were filled by the ALD YSZ.", "Figure 2 (A) Focused ion beam-prepared field emission scanning electron microscopy (FE-SEM) cross-sectional images for 50 nm-thick ALD YSZ films deposited on 80 nm pore AAO supported 40 (left side) and 320 (right side) nm-thick BECs; (B) transmission electron microscopic image for 80 nm pore AAO supported 320 nm-thick BEC.", "Interestingly, the onset point of a voltage plateau for the Cell-B was as low as 0.6 V contrary to that of conventional SOFCs.", "This phenomenon is likely due to the remarkably large activation loss compared to other kinds of losses; the possible reasons for this deactivation are the insufficient electrocatalytic activity of the Pt BEC and the lack of TPB at the electrode–electrolyte interface [15–16].", "The exchange current densities obtained by Tafel fitting were 0.43 mA/cm2 and 0.29 mA/cm2 for the Cell-A and Cell-B, respectively, as shown in Fig. 3 [17].", "Although the values were not significantly different each other, this fitting result indicates that the Cell-A may have somewhat longer TPB length at the BEC side and therefore faster reaction kinetics than the Cell-B, based on the interpretation described in related research [18–19].", "One speculated reason of the longer TPB length for the Cell-A is that more infiltrated ALD YSZ electrolyte into the thinner BEC could have larger BEC–electrolyte contact area, referring to the cross-sectional FE-SEM imaging result of Fig. 2, than the counterpart.", "Figure 3 Tafel plots, measured at 500 °C, for the Cell-A and Cell-B.", "Consequently, the performance comparison and microstructural analysis imply that the thicker BEC elicits higher peak power density due to the superior mass transport through the pores of the AAO substrate in spite of the slightly slower reaction kinetics at the BEC–electrolyte interface.", "Measurements of individual resistances via impedance spectroscopy To investigate the effects of BEC thickness on the individual resistances, electrochemical impedance spectroscopy (EIS) data were obtained for the Cell-A and Cell-B.", "Before comparing the EIS data for two kinds of cells, the EIS curves obtained under different direct current (DC) bias voltages (OCV and 0.1 V with respect to the cathode) for the Cell-B were overlapped to differentiate the ohmic resistance (resulting from charge transport inside electrolyte) from the activation resistance (resulting from reaction kinetics at electrode–electrolyte interface), as shown in the inset of Fig. 4 [20].", "The comparison result indicates that all of the semicircles are relevant to the activation process, i.e., electrode–electrolyte interfacial resistance, not to the ohmic process, i.e., electrolytic resistance, because there are no overlapping semicircles.", "Fig. 4 shows EIS curves obtained under a DC bias voltage of 0.1 V for the Cell-A and Cell-B.", "The EIS curve for the Cell-B contains two predominant semicircles with peak imaginary values at 1 kHz and at 20 Hz by a non-linear least square fitting to the equivalent circuit consisting of one resistance (related to ohmic resistance) and two pairs of constant phase element and resistance (related to electrode–electrolyte interfacial resistance) [6].", "Referring to the previous literatures [6,20–22], it is considered that semicircles at higher and lower frequencies correspond to the anode and cathode interfacial resistances, respectively.", "The Cell-A, on the other hand, shows the EIS behavior with a diagonal form at a lower frequency region below 20 Hz, which is not observed in the impedance spectra of Cell-B.", "This diagonal component is considered to the effect of Waburg element signifying a lack of active fuel supply [13].", "This interpretation corresponds well to the above-mentioned polarization analysis, where we observed a sharp drop in the cell voltage of Cell-A at j > ≈19 mA/cm2.", "The different shape of the semicircle around 20 Hz – which is regarded as the frequency time constant of cathode interfacial resistance [1] – of Cell-A compared with that of Cell-B seems to be due to the overlap of the cathode loop and the Warburg element.", "The high frequency intercept that corresponds to ohmic resistance is 0.5 and 0.45 Ω·cm2 for the Cell-A and Cell-B, respectively.", "Considering both cells have similar cathode sheet resistance of 540–560 Ω·cm and the electrolyte thickness is about the same, such a difference in ohmic resistance may be attributed to a difference in anode sheet resistance stemming from the different thicknesses.", "Nevertheless, this slight difference in ohmic resistance is immaterial to the peak power density of two cells (e.g., a voltage difference between the Cell-A and Cell-B is only 0.5 mV at 10 mA/cm2 that seems to be the range where the ohmic loss becomes dominant).", "Consequently, we think that the mass transport at the anode side needs to be considered as a dominant factor to determine the performance of AAO-supported TF-SOFCs with ALD thin film electrolyte as well as reaction kinetics and ohmic performance.", "Figure 4 Electrochemical impedance spectroscopy analysis results, measured at 500 °C, at bias voltage of 0.1 V for the Cell-A and Cell-B, and (inset) at open circuit voltage and bias voltage of 0.1 V for the Cell-B.", "Experimental Thin film fabrication ALD YSZ film was deposited with a showerhead-type plasma-enhanced ALD machine (Atomic Premium, CN1, South Korea) capable of accommodating one six-inch wafer with a radio frequency plasma generator.", "The processing chamber with a load-lock wafer handler was vacuumized using a dry pump to a base pressure of 2.7 Pa.", "The temperature of the sample stage was set to 250 °C.", "The detailed fabrication process of the YSZ film is presented in our previous work [23].", "PVD YSZ and Pt films were deposited with a sputtering machine (A-Tech System, South Korea) equipped with a custom-designed rotating unit ensuring the high thickness uniformity; the rotating unit was revolved at 4 rpm.", "The target-to-substrate distance was 75 mm, and the substrate was not heated.", "For deposition of the YSZ film, a gas mixture of Ar and O2 in the volumetric ratio of 80:20 was used.", "Background pressure was kept at 1.3 Pa during deposition.", "Radio frequency magnetron power of a sputtering gun was set to 50 W.", "A two inch-sized YSZ disk pellet with an 8 mol % Y2O3 was used as the target.", "For deposition of the Pt film, 99.99% purity Pt disk was used as the target.", "Porous Pt film (for cathode) and much denser Pt film (for anode, BEC) were deposited at 12 Pa and 0.7 Pa, in an Ar gas atmosphere, respectively.", "The DC power of a sputtering gun was set to 200 W, and the purity of Ar gas was 99.99%.", "The fabrication processes of the Pt films are close to the ways described in our preview work [24].", "Thin film characterization The film density was determined by X-ray reflectometry analysis using the X’Pert Pro (PANalytical, Netherlands) instrument.", "The surface microstructure was investigated by FIB/FE-SEM analysis using the quanta 3D FEG (FEI Company, Netherlands) instrument.", "Local surface composition was measured by TEM-EDX analysis using the JEOL-2100F (JEOL, Japan) instrument.", "The characterization techniques utilized in this study are close to the measures described in our preview work [23].", "Electrochemical evaluation Commercial AAO (Synkera, USA) membrane with the thickness of 100 μm and the pore size of 80 nm, as shown in Fig. 5, was used as the porous substrate to support TF-SOFCs.", "Test cells with an active electrode area of 1 mm2 were attached to the custom-designed gas feeding chamber using a ceramic adhesive (CP4010, Aremco Products, USA), which were heated to 500 °C with a ramping rate of 10 °C/min using halogen heaters. 50 sccm dry H2 gas was supplied to the anode side and the cathode was exposed to the atmospheric environment.", "The anode was connected with a combination of silver paste (597A, Aremco Products, Inc., USA) and a 0.5 mm-thick silver wire, while the cathode was contacted using a hardened-steel tip with a radius of 0.19 mm probe moved by a XYZ stage.", "Electrochemical characterization was performed in the two-electrode configuration without a reference electrode.", "EIS analysis was carried out using an electrochemical testing system (1287/1260, Solatron Analytical, UK), in which the alternating current amplitude was set to 50 mV.", "The testing method is close to the way presented in our preview work [6].", "Figure 5 FE-SEM top-view image of AAO membrane with well-arrayed 80 nm-sized pores, cleaned by sonication in ethanol.", "Conclusion We discussed about the preliminary design of BEC for porous AAO supporting TF-SOFCs with conformal and dense thin film electrolyte prepared by ALD technique.", "The thickness of BEC had a significant impact on the infiltration degree of ALD electrolyte into the BEC and the AAO substrate.", "The infiltration degree of ALD electrolyte moderated when the thicker BEC was employed, which led to the generation of appreciably higher peak power density caused by more active mass transport on the BEC side.", "Such thicker BEC improved current collecting performance to some degree; however, resulted in slightly slower reaction kinetics.", "Further optimization of BEC thickness may enhance the cell performance, which could lead to wider potential applications of AAO supporting TF-SOFCs as high-efficiency power sources.", "In addition, the discussion presented in this paper may help to design high-performance porous substrate-supported TF-SOFCs with few hundred nanometer-thick BECs." ]

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[ "In situ fabrication of high-performance Ni-GDC-nanocube core-shell anode for\nlow-temperature solid-oxide fuel cells In situ fabrication of high-performance Ni-GDC-nanocube core-shell anode for low-temperature solid-oxide fuel cells YamamotoKazuhiroa1QiuNan1OharaSatoshib1 1Joining and Welding Research Institute, Osaka University, 11-1 Mihogaoka, Ibaraki, Osaka 567-0047, Japan a k-yamamoto@jwri.osaka-u.ac.jp b ohara@jwri.osaka-u.ac.jp 17433 A core–shell anode consisting of nickel–gadolinium-doped-ceria (Ni–GDC) nanocubes was directly fabricated by a chemical process in a solution containing a nickel source and GDC nanocubes covered with highly reactive {001} facets.", "The cermet anode effectively generated a Ni metal framework even at 500 °C with the growth of the Ni spheres.", "Anode fabrication at such a low temperature without any sintering could insert a finely nanostructured layer close to the interface between the electrolyte and the anode.", "The maximum power density of the attractive anode was 97 mW cm–2, which is higher than that of a conventional NiO–GDC anode prepared by an aerosol process at 55 mW cm–2 and 600 °C, followed by sintering at 1300 °C.", "Furthermore, the macro- and microstructure of the Ni–GDC-nanocube anode were preserved before and after the power-generation test at 700 °C.", "Especially, the reactive {001} facets were stabled even after generation test, which served to reduce the activation energy for fuel oxidation successfully.", "A cermet consisting of the nickel–gadolinium-doped-ceria (Ni–GDC) composite has generated much interest as an attractive anode material for low-temperature solid-oxide fuel cells (SOFCs) because its oxygen ionic conductivity is higher than that of conventional nickel–yttrium-stabilized zirconium (Ni–YSZ) cermet anodes at operating temperatures below 700 °C.", "The oxygen ionic conductivity of GDC (Ce0.9Gd0.1O1.95) has been reported to be approximately 0.01, 0.025, and 0.054 S cm–1 at 500, 600, and 700 °C, respectively1.", "In other words, the diffusion of oxygen ions is seriously inhibited by decreases in the operating temperature.", "Therefore, the effective reaction sites for power generation at low temperatures (500–600 °C) in an anode are confined to areas close to the interface between the solid electrolyte and the anode.", "Some researchers have reported that increasing the triple-phase boundary (TPB) effectively introduced the nanostructures to the electrolyte–anode interface for low-temperature operation2345.", "In general, a conventional SOFC anode is fabricated as follows.", "First, NiO and an oxygen-ion conductor powder are mixed with a binder, after which the anode paste is coated on the electrolyte.", "The anode is then sintered at ∼1300 °C to form the necking structure of anode materials for power generation and collection.", "Finally, NiO is reduced to metallic nickel during the power-generation test67.", "The second step—fabricating the necking structure by high-temperature sintering—is regarded as the essential process.", "However, it prevents the insertion of fine nanostructures near the electrolyte–anode interface because of coarsening of the anode materials.", "Thus, a new process without high-temperature sintering would allow insertion of fine nanostructures, which would help realize the fabrication of anodes that remain stable before and after the power-generation test.", "We have reported organic-ligand-assisted hydrothermal synthesis of ceria and GDC nanocubes covered with highly reactive {001} crystal facets891011, which are considered an attractive catalyst and a good oxygen-ion conductor, respectively.", "In the study reported here, we examined direct fabrication of a Ni–GDC-nanocube cermet anode by chemical reaction in a solution.", "The anode material had a unique core–shell structure composed of 100–200-nm spherical Ni-metal particles covered with 10 nm GDC nanocubes.", "After screen printing of the anode paste on the solid electrolyte, a power-generation test was performed directly without any sintering.", "Through the growth of just a few crystals of Ni spheres, a Ni metal framework for electrical power collection was successfully fabricated during a power-generation test at 500 °C.", "In addition, a vastly enlarged TPB could be inserted near the electrolyte–anode interface without sintering owing to the 10 nm dimensions of fine GDC nanocubes.", "The anode macrostructure, consisting of individual large spherical shapes and a self-fabricated Ni metal framework, provided superior porosity and electrical-power-collection pathways.", "Meanwhile, the reactive nanostructure was attained by controlling the particle size and crystal plane of the oxygen ionic conductor.", "Thus, we could obtain the desired electrode structure through this new strategy for in situ anode fabrication without any sintering.", "The novel fabrication process of a high-performance core–shell Ni–GDC-nanocube anode and its excellent power-generation property are presented here.", "Results All samples prepared by the chemical-reduction method showed multiphase diffraction patterns from face-centered cubic (fcc) nickel metal and CeO2 with a cubic fluorite structure (Figure S1).", "The diffraction peak intensities changed systematically with the initial ratios of Ni to GDC (v:v).", "As shown in Fig. 1a, the sample obtained by chemical reduction in a solution without GDC dispersion (metallic Ni sample) had a spherical morphology, with particle diameters of 100–200 nm.", "On the other hand, the Ni–GDC-nanocube composite sample (Ni:GDC = 65:35) also had a spherical morphology with particle diameters of 200–300 nm, which are slightly larger than the diameters of the metallic Ni particles (Fig. 1b).", "Furthermore, the microstructure of the Ni–GDC-nanocube composite sample was confirmed by detailed observation with transmission electron microscopy (TEM).", "In Fig. 1c, the spherical composite particles with diameters of 200–300 nm had a very fine nanostructure on the surface, and high-resolution (HR)-TEM observation identified that the nanostructure corresponded to the characteristic (002) and (111) lattice fringes of CeO2.", "These results indicate that the Ni–GDC-nanocube composite samples had a core–shell morphology, which consisted of a metallic Ni core covered with GDC-nanocube fine particles measuring 10 nm in size.", "Many researchers have reported synthesis of metallic Ni particles by the chemical-reduction method; the reaction mechanism is summarized as follows121314: Initially, the Ni2+ ions generate a light-blue complex [Ni(N2H4)2]Cl2 with excess hydrazine and the complex precipitates.", "The [Ni(N2H4)2]Cl2 complex is immediately reduced by adding a NaOH solution.", "Very fine metal Ni particles can then easily aggregate owing to van der Waals forces and the magnetism, and such an agglomeration can lead to the crystal growth of metallic Ni particles by Ostwald ripening11.", "In our fabrication process, the [Ni(N2H4)2]Cl2 complex and GDC nanocubes were co-precipitated with hydrazine.", "During the agglomeration and Ostwald ripening, metallic Ni gathered towards the interior as the spherical core and grew to a large sphere measuring 100 to 200 nm in size, while the GDC nanocubes were pushed towards the exterior to cover the metallic Ni sphere.", "After screen printing of the Ni–GDC-nanocube (Ni:GDC = 65:35) paste, the solid-oxide single fuel cells were directly examined to investigate the power-generation properties at temperatures between 500 and 700 °C.", "The voltage–current (V–I) and power–current (P–I) curves are shown in Figure S2.", "Power generation was detected even at 500 °C, which indicates that the anode structure for electrical-power generation and collection was successfully fabricated without any sintering of the anode material.", "Furthermore, higher power densities were obtained at higher operating temperatures.", "The maximum power densities were 25, 51, 97, 158, and 224 mW·cm–2 at 500, 550, 600, 650, and 700 °C, respectively.", "When the power-generation property at 600 °C was compared with that of a NiO-GDC anode that was prepared by an aerosol process followed by sintering at 1300 °C151617, the Ni–GDC-nanocube (Ni:GDC = 65:35) anode showed a maximum power density that was 1.8 times higher (Fig 2).", "In addition, the Ni–GDC-nanocube cermet anode had very high performance that was comparable to that of a NiO–GDC-nanocube compo site anode fabricated by an aerosol process and sintering at 1100 °C11.", "Cross-sectional SEM images of the Ni–GDC-nanocube (Ni:GDC = 65:35) cermet anode before and after the power-generation test at 700 °C are shown in Fig. 3.", "Before the test, the back-scattering image (BSI) shows that the Ni–GDC-nanocube anode consisted of a composite structure of a metallic Ni sphere covered with fine GDC-nanocube particles (Fig. 3a).", "Furthermore, it was confirmed that the macrostructure of the Ni–GDC-nanocube cermet as an electrode, which was established before the power-generation test, remained unchanged even after the test at 700 °C (Fig. 3b,c).", "Meanwhile, the needle-like structures on the surface of the metallic Ni sphere disappeared after the power-generation test.", "The surface morphology became very smooth (Figs 1a and 3c), which means that the in situ fabrication of the metallic Ni framework for electrical power collection resulted from insubstantial crystal growth of the metallic Ni sphere at the operating temperature.", "The cross-sectional mapping images in Fig. 3d, obtained from electron-probe micro-analysis wavelength-dispersive spectroscopy (EPMA-WDX) of the Ni–GDC-nanocube anode after the power-generation test, indicate that the Ni and Ce signals were clearly separated and formed contrasting images.", "Furthermore, the core-shell like morphology did not change even after operating at 600 °C for 24 h (Figure S3a and b).", "It seems that this high stability of novel anode is contributed to the large particle size of Ni spheres and GDC nanocube particles on the surface of Ni spheres.", "Especially, GDC nanocube particles inhibit the crystal growth and migration of Ni spheres.", "These results also confirm the high stability of the anode macrostructure.", "Discussion After analysis of the power-generation properties, the anode material was crushed and its microstructure was closely examined.", "HR-TEM observations revealed that the initial particle size and {001} crystal facets did not change even after the power-generation test at 700 °C (Figure S4), suggesting that the anode macrostructure and the microstructure of the reaction sites produced during the power-generation test could be preserved.", "It should be noted that the macro- and microstructure of the anode fabricated without high-temperature sintering showed good power-generation performance and exhibited very high stability during the test.", "The anode ohmic resistance (ηIRa) and polarization resistance (ηa) at 600 °C were evaluated by the current-interruption method (Figure S5).", "Each ηIRa and each ηa were separated using a Pt reference electrode; the Ni–GDC–nanocube (Ni:GDC = 65:35) anode showed significantly lower ηIRa and ηa than the NiO–GDC anode that was sintered at 1300 °C.", "During the power-generation test at 500–700 °C, the metallic Ni sphere in the Ni–GDC–nanocube (Ni:GDC = 65:35) anode slightly grew in size, and the macro- and microstructure of the anode remained unchanged.", "Ni connection was provided by the slight growing up of Ni sphere; therefore, delamination of the anode layer did not occur.", "It is clear that the enlarged TPB introduced by fine GDC-nanocube particles contributed to the considerable reduction in ηa, which is supported by the SEM images (Fig. 3b–d).", "On the other hand, it is very interesting that the non-sintered Ni–GDC-nanocube (Ni:GDC = 65:35) anode exhibited obviously lower ηIRa than that of the anode sintered at 1300 °C.", "Electromotive forces using only the metallic Ni sphere as an anode in the power-generation test were present because the contact points between the electrolyte and metallic Ni sphere performed as a TPB.", "The fine GDC-nanocube particles on the metallic Ni sphere provided many of these contact points, and this enlarged oxygen ion pathway can be regarded as a reason for the considerable reduction in ηIRa.", "Therefore, it was suggested that the Ni–GDC-nanocube anode could introduce many ultra-fine contacts to the electrolyte–anode interface as well as the anode functional layer234.", "Figure 4 shows Arrhenius plots of the area-specific resistance (ASR or Rsp) of the Ni–GDC-nanocube at 500–700 °C (each impedance spectrum is shown in Figure S6).", "The activation energy (Ea = 50.8 kJ mol–1) of the Ni–GDC (65:35) nanocube anode is much smaller than those of the Ni–GDC anode sintered at 1300 °C11.", "In this study, the fraction of surface diffusion appeared to be very large compared with anodes sintered at high temperature owing to the use of 10-nm GDC nanocube particles as an oxygen-ion conductor.", "Therefore, we assume the apparently low activation energy and Rsp contributed to the increase in reactive {001} facets.", "As the GDC nanocube particles were not sintered and did not have contact with each other (Fig. 3b,c, and Figure S3a and b), the allowable oxygen ion pathway length was considered to be very short because of the rather low oxygen-ion conductivity at 600 °C, despite the high power density shown by the single cell with the 20-μm-thick anode.", "The high power density means that a highly effective electrical pathway was formed along the electrolyte–anode interface to the edge of the anode (electrical collection point).", "To confirm this supposition, a power-generation test was carried out at 600 °C using a 2-μm-thick anode.", "We successfully obtained a high power density that was almost the same as that obtained with a 20-μm-thick anode (Figure S7a–c), indirectly supporting the assumption that the oxygen diffusion distance was quite short (<2 μm).", "These results suggest that novel electrode structure design, which differs from the design for operation at high temperatures, is crucial for low-temperature operation.", "We have demonstrated a novel fabrication process of high-performance Ni–GDC-nanocube anode for low-temperature SOFCs, using only a solution-based chemical reaction.", "The anode material had a core–shell structure, and the core was a metallic Ni sphere that was covered with highly reactive GDC nanocubes.", "The characteristic composite structure could introduce a much longer electrical pathway (>20 μm) without any sintering.", "The effective framework of a metallic Ni sphere was formed by means of crystal growth of metallic Ni spheres during the power-generation test at a temperature as low as 500 °C.", "Meanwhile, the non-sintering fabrication process introduced an enlarged TPB with 10-nm GDC nanocube particles near the interface between the electrolyte and the anode.", "Such micro- and macrostructure of the anode could considerably reduce ηIRa and ηa, and the anode showed great stability even after the power-generation test at 700 °C.", "We conclude that the Ni–GDC-nanocube cermet anode is a suitable anode material for next-generation low-temperature SOFCs.", "Methods Details of organic-ligand-assisted hydrothermal synthesis of GDC (Ce0.9Gd0.1O1.95) nanocubes are described in our previous paper11.", "After hydrothermal treatment, the GDC-nanocube precipitates were washed with distilled water and ethanol.", "The specimen was dispersed in ethylene glycol (EG), and the GDC concentration corresponded to 0.1 M.", "Similarly, NaOH was also dissolved in EG and the concentration was adjusted to 1 M.", "NiCl2·6H2O and the GDC dispersion were added to the EG solvent, and the mixture was heated at 80 °C with stirring.", "N2H4·H2O was slowly released dropwise into the mixture, while the NaOH solution was added rapidly.", "After the mixing bar was removed, the mixture was heated at 80 °C for 2 h.", "The molar ratios of Ni2+:N2H4:NaOH were fixed at 1:20:3.", "The ratios of other components are summarized in Table S1.", "After heating, aggregated dark grey or black precipitates were collected with a neodymium magnet and then carefully washed with distilled water and ethanol.", "The powder was dried at 60 °C for 24 h and mixed with PEG#400 as a binder, and the resulting paste was used as an anode for solid-oxide single-fuel-cell fabrication.", "The solid electrolyte comprised a GDC disk that was sintered at 1500 °C for 4 h (thickness: 400 μm; diameter: 15 mm).", "The La0.6Sr0.4Co0.2Fe0.8O3-δ (LSCF) cathode paste prepared by co-precipitation method was deposited by screen printing on the GDC disk, and the coated disk was heated at 850 °C for 2 h.", "The anode paste was also deposited on the flip side of the GDC disk without post-deposition sintering, and the effective surface area of each electrode was 0.282 cm2 (diameter: 6 mm).", "Power-generation tests were carried out at 500 to 700 °C, following the same procedures described in Ref. 11.", "Additional Information How to cite this article: Yamamoto, K. et al.", "In situ fabrication of high-performance Ni-GDC-nanocube core-shell anode for low-temperature solid-oxide fuel cells.", "Sci.", "Rep. 5, 17433; doi: 10.1038/srep17433 (2015)." ]

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[ "A High-Performing Sulfur-Tolerant and Redox-Stable Layered Perovskite Anode for Direct Hydrocarbon Solid Oxide Fuel Cells A High-Performing Sulfur-Tolerant and Redox-Stable Layered Perovskite Anode for Direct Hydrocarbon Solid Oxide Fuel Cells DingHanpinga13TaoZetian2LiuShun1ZhangJiujunb4 1School of Petroleum Engineering, Xi’an Shiyou University, Xi’an 710065, China 2Key Laboratory for Advanced Technology in Environmental Protection of Jiangsu, Province, Yancheng Institute of College, Yancheng, Jiangsu Province, China 3Colorado Fuel Cell Center, Department of Mechanical Engineering, Colorado School of Mines, Golden CO 80401, USA 4Energy, Mining & Environment, National Research Council of Canada, Vancouver, BC V6T 1W5, Canada ahding@mines.edubJiujun.zhang@nrc.gc.ca 18129 Development of alternative ceramic oxide anode materials is a key step for direct hydrocarbon solid oxide fuel cells (SOFCs).", "Several lanthanide based layered perovskite-structured oxides demonstrate outstanding oxygen diffusion rate, favorable electronic conductivity, and good oxygen surface exchange kinetics, owing to A-site ordered structure in which lanthanide and alkali-earth ions occupy alternate (001) layers and oxygen vacancies are mainly located in [LnOx] planes.", "Here we report a nickel-free cation deficient layered perovskite, (PrBa)0.95(Fe0.9Mo0.1)2O5 + δ (PBFM), for SOFC anode, and this anode shows an outstanding performance with high resistance against both carbon build-up and sulfur poisoning in hydrocarbon fuels.", "At 800 °C, the layered PBFM showed high electrical conductivity of 59.2 S cm−1 in 5% H2 and peak power densities of 1.72 and 0.54 W cm−2 using H2 and CH4 as fuel, respectively.", "The cell exhibits a very stable performance under a constant current load of 1.0 A cm−2.", "To our best knowledge, this is the highest performance of ceramic anodes operated in methane.", "In addition, the anode is structurally stable at various fuel and temperature conditions, suggesting that it is a feasible material candidate for high-performing SOFC anode.", "Solid oxide fuel cell (SOFC), an electrochemical device that can directly convert chemical energy to electricity, has become a feasible technology for energy-supply due to its high-energy conversion efficiency, wide application range and fuel flexibility12345.", "Normally, a SOFC operated at high temperatures can essentially convert any fuel, such as hydrogen, alcohols, hydrocarbons, or even carbon into electricity6.", "Particularly, when using hydrocarbon fuels such as natural gas to produce electricity, SOFC has been recognized to be the most promising device with high conversion and energy efficiencies.", "As identified, the anode plays a critical role in SOFC performance and durability, particularly when a hydrocarbon is used as the fuel.", "Conventionally, Ni-based composites which give high activity for pure H2 oxidation and also good current collection are most commonly used as the anode materials7.", "However, they also exhibit some disadvantages such as low tolerance to coking (carbon deposition) unless a large amount of steam is added to reform the fuel, vulnerability to sulfur intrinsically existing in natural fuels due to the formation of NiS compound8, and nickel coarsening as well as poor volume stability upon redox cycling.", "To overcome these challenges in maximizing the full advantage of the intrinsic fuel flexibility of SOFC, early efforts have been made to develop alternative anode materials.", "For example, replacing the traditional anode with a Cu-ceria-YSZ composite one has been reported to reduce anode carbon deposition to make the SOFC operation in a range of dry hydrocarbons910.", "However, it was found that the inactive Cu particles with poor catalytic activity could limit the cell performance and also suffer coarsening over time owing to the low melting point.", "In order to obtain a high-performing coking-resistant anode, Zhan et al. introduced a thin catalytic layer of Ru-CeO2 that is placed against the anode side, allowing internal reforming of iso-octane without coking and yielding stable power density of 0.6 W cm−2 at 770 °C11.", "This innovative approach showed promising but expensive.", "Several oxides with a perovskite structure have also been explored as the anode materials, which are mixed ionic-electronic conductors in the reducing condition and catalytically more active than ceria for oxidation of hydrocarbon fuels.", "Perovskites could readily accept oxygen vacancies and contain transition-metal cations in the octahedral sites due to the high tolerance factor against crystal distortion.", "Based on these beneficial factors of perovskites, several oxides, such as La0.75Sr0.25Cr0.5Mn0.5O3 (LSCM)12, La0.33Sr0.67Ti1−xMxO3 (LSTO, M = Fen+, Mnn+, Sc)13, Sr2MMoO6 (SMMO, M = Mg, Fe, Co)81415 and Pr0.8Sr1.2(Co,Fe)0.8Nb0.2O4 (K-PSCFN)16, have been investigated as the potential anode materials.", "These conductive anode materials having high resistance against both coking and sulfur poisoning could show some stability in reducing condition.", "However, these anodes showed some limitations, such as insufficient electrical conductivity and low catalytic activity when compared to those of the conventional Ni-YSZ anode.", "For instance, without a Pd or Ni catalyst, pure LSTO or LSCM anode could not provide reasonable performance in H2 below 900 °C and its catalytic activity toward CH4 oxidation seemed insufficient1718.", "It was also observed that the catalytic pathways for reforming methane during the cell operation could be blocked by the residue (SrCO3 and SrMoO4) on the surface of SMMO anode19.", "In the effort to develop high-performing SOFC anodes, we have synthesized a highly redox-stable ceramic oxide with an A-site deficient layered perovskite structure, i.e.", "(PrBa)0.95(Fe0.9Mo0.1)2O5+δ (PBFM) in this work, and when this material is used for the anode, an outstanding electrochemical activity toward fuel oxidation in a direct hydrocarbon fueled SOFC is achieved.", "Our strategy in the selection of this material is based on the following observations: (1) Perovskites with high tolerance against crystal structure distortion could allow to tailor the material’s chemical stability and also the electrical/catalytic/mechanical properties through doping strategy; (2) Fe-rich perovskite containing mixed-valence Fe2+/Fe3+ redox couple could provide high electronic conductivity even though these redox ions only partially occupy the sub-lattice; (3) Layered perovskite structure could give a high electrical conductivity and the ordered A-cations localizing oxygen vacancies within the rare earth layers, which could make a contribution to the fast oxygen surface exchange/bulk diffusion and catalytic activity towards both hydrogen and hydrocarbon oxidation processes; and (4) Our experiments showed that this PBFM was highly stable upon partial removal of lattice oxygen, and that the use of sixfold-coordinated Mo(VI)/Mo(V) couple at B site could stabilize the material with stronger chemical bond against crude anodic conditions8.", "Results Characterization of PBFM anode Figure 1 shows a single-phase layered perovskite structure of PBFM obtained by firing in air at 1000 °C and subsequently in 5% H2 environment at 900 °C (Fig. 1a, Trace a1 and a2).", "As observed, a pure phased PBFM could not be obtained if the sample was fired only in air, during which a large portion of BaMoO4 as a second phase was produced.", "In this case, a further baking treatment (the sample was calcined at 900 °C in 5% H2) in a reducing atmosphere was found to be needed in order to compromise the new charge-neutrality balance induced by the incorporation of larger Mo6+ ions with higher valence than Fe3+.", "After the treatment, a thermogravimetri analysis (TGA) showed that the substantial lattice oxygen was lost in the phase-formation process (Supplementary Fig. 1).", "The crystal structure of this PBFM material presents two structural features: (1) Pr3+ and Ba2+ ions do not form a solid solution at A-site but are ordered in alternating (001) layers.", "A significant difference in size between the large Ba cation and the small Pr cation results in the formation of alternating [PrO] and [BaO] layers along the c-axis with a stacking sequence of ...", "|BaO|FeO2|PrOx|FeO2| ....; and, (2) oxygen vacancies are mainly located at the [PrOx] plane with a great tendency to form ordered patterns under reducing conditions (Supplementary Fig. 2).", "As a result, a coexistence of Fe ions in octahedral and pyramidal environments in an ordered manner can be observed202122.", "It is believed that the oxygen-ion diffusion in such a doped perovskite can be enhanced by orders of magnitude if a simple cubic crystal can transform into a layered compound with ordered Pr and Ba ions.", "The layered structure could reduce the oxygen bonding strength and provides disorder-free channels for ion motion, resulting in lower activation energy and rapid oxygen surface exchange coefficient.", "As shown in the bright-field TEM image (Fig. 1b), the as-prepared PBFM powder has a smooth surface morphology.", "In Fig. 1c,d, the lattice-resolved high resolution TEM (HRTEM) images of the grain edge show the presence of highly crystalline nature, which corresponds to the (200) crystal plane of the double perovskite structure with a lattice inter-planar spacing of d200 = 0.394 nm.", "The selected area electron diffraction (SAED) pattern of boxed area (A2 in Fig. 1b) confirms the long-range order crystal structure.", "The element contents in the nanoparticles as determined by an energy dispersive X-ray (EDX) analysis equipped in TEM showed the existence of Pr, Ba, Fe and Mo, where Cu and C were from the substrate of sample stage (Supplementary Fig. 3).", "The atomic ratio of Pr, Ba, Fe and Mo was determined to be about 5 : 5 : 9 : 1, which was fairly close to the stoichiometric composition.", "Because the small fraction of 0.1 for Mo ions at B site, the coexistence of A and B site cation ordering might not be observable, even if the phase exists as AA'BB'O6-type structure.", "Furthermore, no chemical reaction can be found when firing a mixture of PBFM and LSGM at 1000 °C in air for 100 hours, indicating a good chemical compatibility (Supplementary Fig. 4).", "The thermal expansion coefficient was measured to be 11.96 × 10-6 1/K, which is very close to that of LSGM, and other commonly used electrolytes (Supplementary Fig. 5).", "In addition, PBFM with A-site cation ordering structure is found to be very stable under fuel conditions.", "The layered perovskite structure can be retained when it is fired in 5% H2/95% Ar at even as high as 1000 °C for 200 hours (Supplementary Fig. 6) while the shift of diffraction peaks can be found.", "Electrical and catalytic properties in various conditions For an oxide-based SOFC anode, in order to obtain a comparable to or better performance than that of conventional Ni/YSZ cermet anode, its electrical conductivity should be sufficient for improved catalytic activity and current collection efficiency.", "Figure 2a shows the electrical conductivity of the PBFM as a function of temperature in air and wet 5% H2, respectively.", "It can be clearly seen that PBFM developed in this work has much high conductivities than those of three other ceramic oxide anodes (LSCM12, LSTO13 and SMMO14), suggesting that PBFM should be a high-performing anode material in terms of electrical conductivity.", "This new PBFM material with A-site cation ordered structure could retain high electrical conductivities of 217 S cm−1 in air and 59.2 S cm−1 in 5% H2 at 800 °C, respectively.", "As shown in Fig. 2b, the X-ray photoelectron spectroscopy (XPS) results indicate that the major oxidation states of Fe and Mo in PBFM are + 3 and + 6, respectively.", "The atomic ratios of Fe3+/Fe2+ and Mo6+/Mo5+ couples are determined to be 2.71 : 1 and 28.76 : 1, respectively, indicating the nature of mixed electronic and ionic conductor.", "In air, hole conduction should be predominant in PBFM with reasonable oxygen ion conductivity induced by the substantial oxygen vacancy concentration present in [PrOx] crystal planes.", "After reduction in 5% H2 for 20 hours at 800 °C, the conductivity of PBFM was found to decrease due to the lowered mean Fe valence, but its oxide ionic conductivity was increased due to more available oxygen vacancies, which was consistent with the TGA result that the substantial lattice oxygen is lost above 400 °C in 5% H2, as shown in Supplementary Fig. 1.", "In order to evaluate the electrode performance in different gas conditions, a symmetric half cell using PBFM material as both working and counter electrodes on a LSGM (La0.9Sr0.1Ga0.8Mg0.2O3) electrolyte was prepared, with an Au paste applied as current collector on the both sides.", "As shown in Fig. 3, the PBFM electrode polarization resistances were measured under open circuit conditions in air, wet hydrogen and wet methane atmospheres and different temperatures.", "It can be seen that the electrode polarization resistances in air are 0.027 Ω cm2, 0.11 Ω cm2, and 0.88 Ω cm2 at 800 °C, 700 °C and 600 °C, respectively, which are comparable to commonly used cathode materials such as La0.8Sr0.2MnO3 (4.2 Ω cm2 at 700 °C)23, and LaxSr1−xCoyFe1-yO3-δ (0.34 Ω cm2 at 700 °C)24, indicating the excellent catalytic activity of PBFM for oxygen reduction reaction.", "As shown in Fig 3, the electrode polarization resistances of PBFM anode in H2 are 0.074, 0.132 and 0.231 Ω cm2 at 800 °C, 750 °C and 700 °C, respectively, which are lower than previously developed oxide anodes.", "For instance, the LSCM anode developed by Tao et al.12 exhibited a polarization resistance of 0.26 Ω cm2 in wet H2 at 900 °C.", "For a recently well-developed Sr2Fe1.5Mo0.5O6 anode, the lowest polarization resistance of 0.21 Ω cm2 was reported at 800 °C in H215.", "Furthermore, this PBFM anode can even give very promising performance when operation temperature is decreased: 0.44 Ω cm2 at 650 °C and 0.93 Ω cm2 at 600 °C, respectively.", "As calculated, the activation energy of PBFM in H2 was 1.02 eV, lower than 1.31 eV in air, indicating an advantage if this material is used for SOFC anode.", "When the gas condition is switched to methane (~3% H2O), the polarization resistance is consequently raised up to 0.86 Ω cm2 at 800 °C, 3.25 Ω cm2 at 750 °C and 10.76 Ω cm2 at 700 °C, respectively.", "Power output and durability of fuel cells in H2, CH4 and H2S-containing H2 Figure 4a shows the electrochemical performance of a LSGM electrolyte-supported SOFC with the configuration of PBFM|LSGM|PBCO (PrBaCo2O5+δ), tested using various humidified (~3% H2O) fuels (H2 and CH4) and ambient air as oxidant.", "It can be seen that the open circuit voltage (OCV) for wet H2 is close to the theoretical value calculated by the Nernst equation, 1.12 V at 800 °C, 1.14 V at 700 °C and 1.16 V at 600 °C, respectively.", "The maximum power density (Pmax) can reach up to 1.72, 1.05 and 0.56 W cm−2 at 800, 700 and 600 °C, respectively, and the cell exhibits a very stable performance under a constant current load of 1.0 A cm−2 at 700 °C for 450 hours without any degradation (Supplementary Fig. 7).", "The OCVs of the cell using wet (3%H2O) methane as fuel can reach to 0.9 V at 800 °C, 0.94 V at 750 °C and 0.97 V at 700 °C, respectively.", "PBFM anode can show a high maximum power density of 0.54 W cm−2 at 800 °C.", "To our best knowledge, this is the highest performance of ceramic anodes operated in methane.", "The impedance spectra measured under open circuit condition with wet H2 and CH4 as fuels are shown in Supplementary Fig. 8.", "It can be seen that the overall electrode polarization resistance is as small as 0.057 Ω cm2 in H2 and 0.255 Ω cm2 in CH4 at 800 °C, respectively, and the long-term durability test shows no obvious degradation when the cell was discharged at 0.5 A cm−2 and 750 °C for 420 hours (Fig. 4b).", "The electrochemical performance of PBFM anode can compare favorably to those of previously reported high-performance of direct hydrocarbon fueled SOFCs with ceramic anodes (Supplementary Table 1).", "Yoo et al.25 reported a maximum power density of ~0.63 W cm−2 in H2 at 800 °C for a LSGM (~250 μm) electrolyte supported SOFC with Ni-impregnated La0.2Sr0.8Ti0.98Co0.02O3-GDC composite anode.", "With La0.3Sr0.7TiO3 anode infiltrated by Pd (0.5 wt%) and CeO2 (5 wt%), the maximum power density was increased to 0.78 W cm−2 at 800 °C26.", "Liu et al.15 reported a cell performance of 0.84 W cm−2 in H2 and 0.23 W cm−2 in CH4 at 900 °C for Sr2Fe1.5Mo0.5O6 anode, and recently, Yang et al.16 reported a very promising cell performance of 0.96 W cm−2 in H2 and 0.6 W cm−2 in CH4 at 850 °C for a K2NiF4-type K-PSCFN-CFA anode with Co-Fe alloy, which were still lower than the performance in this work.", "It should be noted that the thin electrolyte LSGM with thickness of only 200 μm and catalytically active cathode PBCO also contributed to the high performance.", "In the performance optimization, it was found that the electrode polarization resistances could be further improved by optimizing the microstructure of PBFM anode or PBCO cathode.", "In the experiments, a single cell with nanostructured anode microstructure (Supplementary Fig. 9) of the prime backbones infiltrated by the PBFM solution precursors with stoichiometric amounts was fabricated.", "The as-prepared cell shows a further enhanced performance, for example, the power densities of 2.3, 1.5 and 0.8 W cm−2 at 800, 700 and 600 °C in H2 can be achieved, respectively (Supplementary Fig. 10).", "Furthermore, power densities of 0.76 W cm−2 in CH4 and 2.02 W cm−2 in H2-30 ppm H2S at 800 °C can also be obtained.", "These high-performing results demonstrate the great potential of PBFM to be applied as oxide anode in high-performance SOFC operated in various fuels.", "In order to determine the sulfur tolerance of PBFM anode, the cell performance in H2 containing H2S contaminant (H2 + ppm H2S) at different concentrations were tested.", "As shown in Fig. 4c, the maximum power densities of the cell are 1.62, 1.32 and 1.03 W cm−2 at 800, 750 and 700 °C in H2 containing 30 ppm H2S (Fig. 4c).", "In the experiments, when the fuel is switched to H2 + 60 ppm H2S and then H2 + 100 ppm H2S, the values of Pmax can still maintain at 1.25 and 1.18 W cm−2, respectively, as seen in Supplementary Fig. 11.", "The cell under a constant current load of 1.0 A cm−2 exhibits a very stable durability in H2 + 30 ppm H2S at 750 °C, with a very small voltage drop in 520 hours (Fig. 4d).", "To examine the performance response to the fuel change, the cell with the PBFM anode was also examined when the fuel was switched between H2 and CH4.", "As shown in Supplementary Fig. 12, a constant current density of 0.8 A cm−2 is applied at 750 °C with monitoring the cell voltage change.", "It can be seen that a sharp decrease in cell voltage from 0.89 V to 0.3 V can be observed after the fuel is switched from wet H2 to CH4 due to the lower catalytic activity of PBFM anode for CH4.", "The cell voltage can be immediately recovered to a slightly higher value of 0.9 V after the fuel gas is switched from CH4 back to wet H2.", "Similar behavior can also be observed when the fuel gas is switched between wet H2 and H2 + 100 ppm H2S.", "These results demonstrate that the PBFM anode has a fast response and recovery ability to the fuel change and contamination.", "Redox stability of PBFM anode Normally, the poor redox tolerance of nickel cermet anode can preclude many medium- and small-scale applications, caused by a volume instability.", "Therefore, redox cycling stability is another critical aspect in evaluating an anode material’s performance for SOFCs, which is tested by switching the fuel gas between H2 and air at the anode side.", "As shown in Fig. 5a, the cell is initially operated under a constant current load of 0.7 A cm−2 in H2 at 600 °C for 3 hours to obtain a stable cell performance as baseline.", "Subsequently, the PBFM anode is subjected to the first redox cycle by sweeping air for 0.5 hour and then back to H2 for other 0.5 hour.", "It can be seen that the current density is firstly dropped to 0 V upon oxidation and then quickly recovered to initial value and stabilized.", "After five redox cycles, there is no any degradation on cell voltage.", "In addition, the impedance spectra of the fuel cell are also measured before and after the redox cycles, as shown in Fig. 5b.", "It can be seen that the major impact of redox cycling is on the value of electrode polarization resistance (with a slight decrease) rather than on the ohmic resistance, demonstrating that this anode material has a remarkable redox stability.", "As shown in Supplementary Fig. 13, the microstructure of post-test cells is also examined by scanning electron microscopy, showing a good adhesion between two ceramic layers.", "Discussion Regarding the roles of Fe and Mo in the perovskite materials, Goodenough and Huang27 and Lindén et al.28 indicated that it might not be possible to reduce all the Fe3+ ions completely to Fe2+ in recently developed anode material of Sr2FeMoO6 because the Mo5+/Mo6+ redox band overlaps with the Fe2+/Fe3+ couple, therefore protecting the Fe3+ in the perovskite structure from being fully reduced.", "This is consistent with our results that the crystal structure of PBFM could show a high resistance against reducing condition.", "It is worthwhile to note that the strategy of material selection in this work is distinguished from conventional exploration of oxide anodes for SOFCs.", "The most popularly used LSCM and LSTO anodes are developed on the basis of obtaining the stable crystal in both reducing and oxidizing atmospheres due to highly tolerant TiO6 or CrO6 octahedra with preference of six-fold coordination in its chemistry29.", "For example, LSCM is originated from the ceramic interconnect material of LaCrO3, which is stable and conductive in both fuel and air conditions.", "To make them workable for SOFC anodes, doping strategy is generally adopted to gain reasonable ionic and electronic conductivity for electrochemical reactions.", "The replacement of a stable B-site ion by another active element, for example, Mn partially replacing Cr, Co partially replacing Ti, would create a new material that compromises between stability and activity while the two elements act in a complementary fashion.", "On the contrary, the active material might be stabilized with partially replacement of stable element while the structural, electrical and catalytic properties may be maintained to the largest extent.", "In this regard, conventional multivalent elements (Mn, Fe, Ni, etc.) could not only serve to compensate the creation of oxygen vacancy and function as charge carriers for electrons or holes, but also give certain stability in weak reducing condition30.", "Some typical examples include the La0.7Sr0.3FeO3-δ31 and Ba0.95La0.05FeO3-δ32 for oxygen permeation and membrane conversion.", "In order to stabilize the structure of these active perovskites, some elements such as Ti, Cr or Mo may be used to partially dope B-site.", "For layered perovskite PrBaFe2O5+δ, when 10% B-site cation is replaced by Mo, the crystal structure could become very resistant against H2 from extrusion of metal elements, and also contain necessarily adequate charge carriers for electrochemical reactions.", "For PBFM developed in this work, the XPS analysis discussed above can validate the coexistence of Fe3+/Fe2+ and Mo6+/Mo5+ couples with content ratios of 2.71 : 1 and 28.76 : 1, respectively, which are believe to be able to make a contribution to both conductivity and stability (Fig. 2).", "In 5% H2, the retained electrical conductivity demonstrates the availability of charge carriers in a broad range of oxygen partial pressure, which is comparable to other Ni-free oxide anodes, such as La0.3Sr0.7TiO3-δ33, La0.7Sr0.3VO334 and Ba2FeMoO6-δ35, and higher than both La0.6Sr0.4Fe0.9Mn0.1O336 and PrBaMn2O5+δ37 (Supplementary Table 2).", "As a mixed ionic-electronic conducting anode, on the other hand, the anode performance should also strongly depend on oxygen self-diffusion (D*) and surface exchange rate (k*).", "These two processes could allow the electro-oxidation process to extend from three-phase electrode/electrolyte/gas boundary to the anode surface, then leading to a catalytic enhancement.", "In this regard, Tarancón et al.38 suggested that low electrode polarization resistance could be achieved with requirements of k*D* > 10−14 cm3s−2 and k*/D* < 100 cm−1.", "As believed, the special structural feature of layered perovskite may be able to facilitate rapid oxygen mobility and surface exchange in PBFM anode.", "The anisotropy of oxygen diffusion due to the presence of A-site cation ordered structure with alternating AO6/2 and A'O6/2 top-corner-shared octahedra may be significantly enhanced, where the rich oxygen vacancies are mainly located in the rare earth planes along the a axis.", "For example, Taskin et al.22 investigated the re-oxidation kinetics of GaBaMn2O5+δ and GaBaCo2O5+δ in which the A cation lattice could be ordered or disordered depending on the synthesis process, and found a remarkable enhancement of oxygen diffusion at rather low temperatures, exceeding 10−5 cm2/s at 600 °C.", "Kim et al.21 applied the isotopic diffusion measurements on PrBaCo2O5+δ and reported high values of D*, e.g. > 10−7 cm2 s−1 at 500 °C, despite the porosity of only 90% could give rise to an overestimated value.", "Furthermore, the porous thin layer of PBFM (~10 μm) might also facilitate the minimization of polarization resistance.", "In conventional Ni-YSZ cermet anode, Ni can provide high electrical conductivity for electron transport in the process of reaction and also current collection in the thick substrate.", "For PBFM anode, the thin layer should be able to relieve the suffering of relatively lower conductivity for the same purposes.", "Furthermore, the advantage of perovskite anodes also includes the oxygen-rich structure, which could tolerate the loss or gain of lattice oxygen when subjected to change of gas conditions, which might be ascribed to high-coordination BO6 octahedra.", "The rapid recovery of current density when the gas was switched from air to H2, as discussed above, indicates that the non-stoichiometry of PBFM should be able to promptly change to original value for recurrence of properties.", "In summary, PBFM has therefore been demonstrated as a novel ceramic oxide anode with A-site cation-ordered layered perovskite structure, which shows high electrochemical performance in various fuel conditions.", "The excellent redox stability and high resistances against both coking and sulfur poisoning are concept-of-proof indicative of that the high catalytic activity for fuel electro-oxidation can be well kept at moderate temperatures in the absence of excess steam.", "It is also evidently suggested that performance can be further improved by the optimization of microstructure of both electrodes.", "In addition, this PBFM anode could greatly facilitate its application in anode-supported fuel cells, when some technical strategies, such as introducing some electrically conductive metal-phase materials into anode structure, are required to improve the total anode conductivity and catalytic activity.", "Methods Layered perovskite oxide of (PrBa)0.95(Fe0.9Mo0.1)2O5+δ(PBFM) was synthesized using modified Pechini process39, where citrate and ethylene diamine tetraacetic acid (EDTA) were employed as parallel complexing agents.", "In the synthesis, Pr6O11 was first dissolved in nitric acid; the calculated amounts of Ba(NO3)2, Fe(NO3)3·9H2O and Mo7(NH4)6O24∙4H2O were dissolved in EDTA-NH3 aqueous solution under heating and stirring conditions.", "An appropriate amount of citric acid was then added into the solution.", "After converted into a viscous gel under heating and stirring conditions, the solution was ignited to flame and resulted in an ash-like material.", "Then, this ash-like material was calcined in air at 1000 °C for 10 hours and then in 5% H2 at 900 °C for 5 hours to obtain the final material (PBFM).", "The phase structure of PBFM was analyzed by X-ray powder diffraction by Cu-Kα radiation (D/Max-gA, Japan).", "A scan rate of 1 ° min−1 was used in the range of 20 ° < 2θ < 80 °.", "The anode particles were analyzed by transmission electron microscopy (TEM, JEOL 2100F) operating at 200 kV equipped with energy-dispersive X-ray spectroscopy (EDX) to obtain the details about crystal lattice, element distribution and selected area electron diffraction pattern.", "XPS was conducted on a Kratos Axis Ultra DLD instrument.", "Thermogravimetric analysis (Netzsch STA 449) was performed at 25-900 °C with a heating/cooling rate of 2 °C min−1 in air or 5% H2 to characterize the loss process of lattice oxygen.", "The rectangular bar of PBFM was cold pressed and consequently sintered at 1300 °C for 10 h to form dense pellet with relative density of 95%.", "Electrical conductivity of the PBFM was measured as a function of temperature using a direct current four-probe technique (Agilent 34001A) in air and 5% H2, respectively.", "The area-specific-resistance (ASR) values were measured using a symmetric cell PBFM|LSGM|PBFM in dry air, humid H2 and CH4 (~3% H2O) separately, at different temperatures.", "The full fuel cells with layered PBFM as anode and cobalt-containing layered oxide PrBaCo2O5+δ (PBCO) as cathode were prepared based on LSGM electrolyte support.", "The electrode inks consisting of PBFM (or PBCO) were then applied to the either side of the LSGM electrolyte by brush painting, and then fired at 1000 °C in air for 5 hours to form a porous anode and cathode, respectively.", "The resulting electrode had a thickness of ∼ 10 μm and an effective area of 0.25 cm2.", "The button cells were sealed onto a home-made alumina tube using a sliver paste.", "The cells were tested from 600 to 800 °C with the static air as oxidant and humid hydrogen (~3% H2O), methane or H2S-containing H2 as fuel with a flow rate of 80 ml min−1.", "The voltage-current curves were recorded by DC load at a scanning rate of 50 mV s−1.", "The electrochemical impedance spectra were obtained over a frequency range from 0.01 to 105 Hz under the open-circuit conditions using an electrochemical station (Zennium ZAHNER).", "A field-emission scanning electron microscope (JSM-6301F) was used to observe the microstructure of the post-test cells.", "Additional Information How to cite this article: Ding, H. et al.", "A High-Performing Sulfur-Tolerant and Redox-Stable Layered Perovskite Anode for Direct Hydrocarbon Solid Oxide Fuel Cells.", "Sci.", "Rep. 5, 18129; doi: 10.1038/srep18129 (2015)." ]

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[ "Proton-conducting Micro-solid Oxide Fuel Cells with Improved Cathode Reactions by a Nanoscale Thin Film Gadolinium-doped Ceria Interlayer Proton-conducting Micro-solid Oxide Fuel Cells with Improved Cathode Reactions by a Nanoscale Thin Film Gadolinium-doped Ceria Interlayer LiYong1WangShijie2SuPei-Chena1 1School of Mechanical and Aerospace Engineering, Nanyang Technological University, 50 Nanyang Avenue, Singapore 639798 2Institute of Materials Research and Engineering, Agency for Science, Technology and Research (A*STAR), 2 Fusionopolis Way, Singapore 138634 apeichensu@ntu.edu.sg 22369 An 8 nm-thick gadolinium-doped ceria (GDC) layer was inserted as a cathodic interlayer between the nanoscale proton-conducting yttrium-doped barium zirconate (BZY) electrolyte and the porous platinum cathode of a micro-solid oxide fuel cell (μ-SOFC), which has effectively improved the cathode reaction kinetics and rendered high cell power density.", "The addition of the GDC interlayer significantly reduced the cathodic activation loss and increased the peak power density of the μ-SOFC by 33% at 400 °C.", "The peak power density reached 445 mW/cm2 at 425 °C, which is the highest among the reported μ-SOFCs using proton-conducting electrolytes.", "The impressive performance was attributed to the mixed protonic and oxygen ionic conducting properties of the nano-granular GDC, and also to the high densities of grain boundaries and lattice defects in GDC interlayer that favored the oxygen incorporation and transportation during the oxygen reduction reaction (ORR) and the water evolution reaction at cathode.", "Micro-solid oxide fuel cells (μ-SOFCs) using nanoscale thin film electrolytes have shown a great promise as portable power sources because of their high performance at drastically reduced operating temperatures1.", "By minimizing the electrolyte thickness from tens of micrometers scale down to sub-micrometer scale, Ohmic resistance of conventional oxygen ion-conducting electrolytes such as yttria-stabilized zirconia (YSZ) decrease proportionally with thickness, which enable the high cell performance at temperatures lower than 500 °C234567.", "As Ohmic resistance is minimized, the most rate-limiting process among the entire cell reactions is shifted to the cathode polarization, since the thermally-driven oxygen reduction reaction (ORR) kinetics at the cathode becomes much more sluggish at such low temperature range8.", "Therefore, improving the kinetics of cathodic reactions or the selection of catalytically more active cathode materials is currently the most critical issue in further enhancing the performance of such promising devices.", "Among reported μ-SOFCs, quite a few works have shown impressive performance using oxygen ion-conducting electrolytes such as YSZ, gadolinium-doped ceria (GDC), or with multiple-layer configurations like GDC/YSZ bilayer electrolyte25.", "However, for μ-SOFCs operating at their targeted temperature regime, which is usually below 500 °C, proton-conducting oxides can be more suitable choices as electrolyte materials since they usually possess better ionic conductivity than oxygen-ion conductors at low temperature due to lower activation energy of proton conduction9.", "It should be expected that the already impressive performance of μ-SOFCs reported can be further improved if the oxygen ion-conducting electrolyte is replaced with proton-conducting electrolyte while remaining the other cell components such as porous metal catalytic electrodes unchanged.", "Nevertheless, to date, among the limited number of reports on μ-SOFCs using the most common proton-conducting electrolytes (μ-H-SOFCs hereafter) like yttrium-doped barium zirconate (BZY), the peak power densities reported were still much lower than those using zirconia- or ceria-based oxygen ion-conducting electrolytes (μ-O-SOFCs hereafter).", "As summarized in Table 1, the highest peak power densities attainable for μ-H-SOFCs were only 140 mW/cm2 at 400 °C10 and 186 mW/cm2 at 450 °C11.", "For the reported high performance of μ-O-SOFCs, the highest peak power densities reported were closer to or over 1 W/cm2 at 450 °C456.", "The lower performance of μ-H-SOFCs may originate from the poor cathode configuration that provides insufficient reaction sites on such type of nano thin film fuel cells.", "Figure 1a shows the typical cathode/electrolyte/anode cross-sectional schematics of the μ-H-SOFC, which has a nano thin film BZY electrolyte sandwiched between two porous thin film Pt electrodes.", "Unlike conventional SOFCs, the cathode/electrolyte interface of a μ-SOFC is only connected two-dimensionally, which means the triple phase boundary (TPB) for the ORR is only limited to the planar interface between Pt cathode and oxide electrolyte.", "When the electrolyte is changed from an oxygen ion conductor to a proton conductor, in addition to the existing ORR, the water evolution reaction also shifts from anode to cathode, making the complex cathode reactions even more complicated.", "In BZY μ-H-SOFCs, the reduced oxygen ion may only meet the proton transported from the anode through BZY near the TPB lines at the interface between Pt cathode and BZY (red line in Fig. 1a), and these are the likely places where the water evolution reaction occurs.", "Therefore, it is expected that the performance of μ-H-SOFCs has been limited by the confined reaction zone that resulted in high cathodic polarization resistance.", "In this regard, modifying the interface between Pt and BZY to allow the cathodic reactions to take place over an extended zone is expected to effectively improve the cathode kinetics and increase the cell power performance.", "Among studies for regular proton-conducting electrolyte SOFCs (H-SOFCs) operated at intermediate temperature range (500 to 650 °C), the search of suitable cathode materials to accommodate the complex cathode reactions is also a prevailing topic12131415.", "One of the most promising categories of cathode is triple-conducting materials, which are materials having simultaneous electronic, oxygen ionic, and protonic conduction properties16.", "A triple-conducting cathode provides more reaction sites for both the ORR and water evolution reaction to take place that is believed to effectively decrease the cathode polarization resistance, and the reported cell performances using such cathode material are indeed impressive13.", "To apply such concept to μ-H-SOFCs, adding an interlayer between the cathode and electrolyte, or the so-called bi-layered electrolyte, can be an effective method.", "For μ-O-SOFCs, the concept of bi-layered electrolytes or the cathode/electrolyte interface modifications have been demonstrated to effectively improve the cathode kinetics.", "A catalytically superior material for ORR, such as doped-ceria2517, can be inserted between the porous metallic cathode and the main electrolyte to serve as a good cation diffusion barrier18 and improve the ORR reaction kinetics1920.", "Results from quantum mechanical simulation also showed very low oxygen incorporation energetics, of 0.07 eV for doped ceria at cathode/electrolyte interface, which is much lower than the 0.38 eV of YSZ21.", "To apply the bi-layer electrolyte concept to μ-H-SOFCs for better cathode reaction kinetics, GDC can still be a good choice to accommodate the complex cathode reactions.", "The Ga doping in ceria gives the higher oxygen diffusion coefficient than ceria doped with other dopants such as Y, Sm, and La22.", "More importantly, evidences of proton conduction at temperature lower than 400 °C were also reported23242526.", "The mixed oxygen ion and proton-conducting property allows both the oxygen ions and protons to transfer into the GDC layer, and therefore it is likely to extend the water formation and evolution zone from the confined TPB lines (Fig. 1a) into part of or the entire GDC layer (Fig. 1b).", "Therefore, the purpose of this work is to demonstrate the concept of adding a GDC interlayer which is catalytically more active and is a mixed oxygen ionic and protonic conductor, in order to improve the chronically poor performance of μ-H-SOFCs.", "An 8 nm-thick GDC layer was deposited on top of BZY proton-conducting electrolyte to serve as a cathode interlayer for μ-H-SOFCs.", "Cathode performance and fuel cell power density in the silicon-based μ-H-SOFC were significantly improved with the addition of GDC interlayer.", "The electrochemical impedance and fuel cell performance of the fabricated μ-H-SOFCs with and without the GDC interlayer were characterized to understand the effect of such cathode interlayer on the cathode kinetics behavior.", "Results Microstructure of the GDC/BZY Electrolyte Figure 2 shows the XRD patterns of BZY electrolyte with and without GDC cathodic interlayer.", "The BZY electrolyte layer has a polycrystalline structure with a preferred orientation of (011).", "All of the peaks were indexed to the standard BZY PDF card 96-720-2180, which indicates well-crystallized BZY film at the deposition temperature of 800 °C.", "In the case electrolyte with GDC interlayer, additional GDC peaks were clearly observed and well-matched with the standard GDC pattern of PDF 00-046-0508.", "The relatively low intensity of GDC peaks was due to the much smaller thickness of GDC interlayer (8 nm) than BZY (75 nm).", "No additional phase was observed from the bi-layer electrolyte, which means there is no reaction between BZY and GDC during the deposition at 800 °C.", "The FESEM cross-sectional images of both the μ-H-SOFCs having the BZY electrolytes with and without GDC interlayer are shown in Fig. 3.", "The dense BZY electrolytes in both cases were 75 nm in thickness and sandwiched between the porous Pt cathode and anode of 100 nm and 60 nm in thickness, respectively.", "Cross-sectional TEM characterizations were performed for GDC/BZY bi-layer electrolyte to investigate the crystallinity and the microstructures (Fig. 4).", "Both of the fully crystallized BZY electrolyte and GDC interlayer showed columnar grains with vertical grain boundaries parallel to the ion transportation direction (Fig. 4a), which can minimize the cross grain boundary resistance during proton conduction27.", "The thickness of BZY electrolyte and GDC interlayer were confirmed to be 75 nm and 8 nm, respectively (Fig. 4b).", "No additional phase was visible between the BZY and GDC layers, which suggests good chemical compatibility and stability between these two layers at the deposition temperature of 800 °C, and this is in agreement with the XRD results.", "Therefore, no reaction is expected to occur during the μ-H-SOFC operation because of the much lower operating temperature (below 500 °C) than the deposition temperature.", "Although a large mismatch of lattice constant exists between BZY (0.42 nm) and GDC (0.54 nm), the grain boundaries of the GDC interlayer were aligned to the grain boundaries of the underneath BZY during the grain growth from PLD deposition.", "The grain alignment introduced a compressive stress to the GDC interlayer, which resulted in a high density of dislocations and lattice distortion, as shown in Fig. 4c.", "The dislocations were not only present at the vicinity of GDC/BZY interface, but also extended through the GDC grains.", "The inversed fast Fourier transform (FFT) image in Fig. 4d clearly shows the existence of dislocations and lattice distortion by the compressive strain between BZY and GDC layers.", "Electrochemical Characterization Figure 5 shows the polarization curves for μ-H-SOFCs using BZY electrolytes with and without the GDC cathode interlayer.", "Both fuel cells showed stable and high open-circuit voltages (OCVs) in the range of 0.98 to 1.07 V close to the theoretical thermodynamic value of 1.1 V, indicating that dense and pinhole-free electrolytes remained intact during the cell operation.", "The peak power densities obtained from the cell using BZY-only electrolyte were 51, 93 and 206 mW/cm2 at 350, 375, and 400 °C, respectively.", "For the cell with GDC interlayer, the peak power densities further increased up to 106, 187, 274 mW/cm2 at 350, 375, 400 °C, and reached 446 mW/cm2 at 425 °C.", "The peak power density values of both the cells with and without GDC interlayer were all higher than the reported values of μ-H-SOFCs at the same testing temperatures, as summarized in Table 1.", "To confirm the improved reaction kinetics at the cathode side, the EIS curves of both the cells with and without the GDC interlayer were studied at 350 to 400 °C (Fig. 6).", "The first intercept on the real axis at high frequencies represents the Ohmic resistance RΩ, and the second intercept on the real axis at low frequencies corresponds to the total resistance of the cell28.", "For the polarization resistance Rp, two distinguished arcs can be identified, where one has the characteristic frequency at the high frequency range (HF, ~105 Hz) and the other at medium frequency range (MF, 102–103 Hz).", "The EIS curves were fitted using the equivalent circuit model of two parallel R and CPE (constant phase element) and one resistor connected in series, as shown in the inset of Fig. 6.", "The values extracted from the curve fitting were summarized in Table 2.", "The values of (R1, CPE1) and (R2, CPE2) corresponded to the HF and MF arcs, respectively.", "Each CPE has a CPE-T, which is related to the relaxation capacitance, and a CPE-P, which reflects the displacement of the center of the arc from the real axis29.", "As summarized in Table 2, total polarization resistances Rp of the cell without GDC interlayer were 11.899, 7.045, and 3.660 Ωcm2 at 350, 400, and 450 °C, respectively, while the cell with GDC interlayer decreased to 4.136, 3.346, and 2.443 Ωcm2 at 350, 400, and 450 °C, respectively.", "The decrease in Rp indicates that the cathodic reaction was promoted by the additional GDC interlayer.", "Since the electrolyte and electrodes were identical for both cells across all experiments, the changes in Rp should be due to the presence of GDC interlayer.", "Ohmic resistances of the BZY electrolyte cell were 0.085, 0.089, and 0.099 Ωcm2, and for the GDC/BZY cell, the resistances increased slightly to 0.115, 0.129, and 0.131 Ωcm2 at 350, 375, and 400 °C, respectively, likely due to the additional thickness from GDC and the interface between GDC and BZY.", "The variations in the Ohmic resistance between these two cells can be negligible since they are relatively small as compared to the value of polarization resistance Rp.", "Discussion The improved cathode kinetics by the GDC interlayer can be identified from the corresponding Bode plot of each EIS curve (Fig. 6c).", "Two rate limiting steps were observed for both cells with and without GDC interlayer: the proton migration from the electrolyte to the TPBs, which corresponds to the HF resistance, and the oxygen dissociative adsorption and diffusion, which is related to the MF resistance16.", "With the GDC interlayer, MF resistances were decreased from 7.179, 4.582, and 2.557 Ωcm2 to 2.485, 2.070, and 1.776 Ωcm2 at 350, 375, and 400 °C, respectively, corresponding to the slightly depressed MF arc in the Bode plot with a frequency shift from 102 Hz to 103 Hz.", "The reduction in MF resistance means an enhancement in oxygen dissociative adsorption process on the GDC surface, which may originate from the high density of grain boundaries and dislocations in the GDC interlayer that provide preferential oxygen incorporation sites for lower interface resistance and faster surface exchange kinetics303132.", "The HF peaks in the Bode plot of the cell with GDC interlayer showed more apparent depression than that of the cell with only BZY electrolyte at all testing temperatures, indicating the enhancement of charge transfer process across the cathode/electrolyte interface in the presence of the GDC interlayer.", "The HF polarization resistances of the cell without GDC interlayer were 4.720, 2.463, and 1.103 Ωcm2 at 350, 400, and 450 °C, respectively, and the cell with GDC interlayer decreased to 1.651, 1.276, and 0.997 Ωcm2 at 350, 400, and 450 °C, respectively.", "The enhanced charge transfer process originated from the mixed conduction of proton and oxygen ion in the GDC layer, which can extend the reactions sites for water formation and evolution process.", "As depicted in Fig. 1b, the dissociative adsorbed oxygen ions can transfer from TPBs and surface grain boundaries to the GDC interlayer through oxygen vacancies.", "When proton reaches to the GDC/BZY interface, it can migrate to the GDC interlayer and react with the oxygen ions present within the GDC interlayer.", "Thus, the active regions involved in facilitating the water formation and evolution are not limited to the interface between Pt cathode and electrolyte, but extended to the GDC interlayer such that the HF resistance was decreased.", "Although the exact ORR and water evolution reaction mechanisms and pathways within the interlayer are still unclear, it is evident that the combined conduction of both O2- and H+ has effectively improved the cathodic kinetics, leading to enhanced fuel cell performances at low temperature range for proton-conducting SOFCs.", "In summary, the complex cathodic reactions in a μ-H-SOFC using BZY electrolyte were studied by an interface modification with the addition of an 8 nm-thick GDC cathode interlayer.", "The cathodic polarization resistance was effectively decreased by the additional GDC interlayer between the Pt cathode and BZY electrolyte.", "A record high peak power density of 445 mW/cm2 was obtained at 425 °C from the μ-H-SOFC with GDC/BZY bi-layer electrolyte.", "The EIS analysis of cathodic impedance of the fuel cells showed the enhanced cathodic charge transfer process across the cathode/electrolyte interface with the help of GDC interlayer, suggesting the effective promotion of proton and oxygen ion charge transfer as well as ORR and water evolution reaction between Pt cathode and BZY electrolyte through the GDC interlayer.", "The mixed oxygen and proton conduction in the GDC interlayer expanded the cathodic reaction sites from a 2-dimentional planar interface between Pt and BZY to nearly the entire GDC interlayer.", "The findings in this work show that cathodic interfacial resistance indeed has suppressed the possible high performance of μ-H-SOFCs.", "Further study on fundamental mechanisms into the protonic and oxygen ionic conduction pathways and reaction mechanism within the cathodic interlayer deserves an extensive exploration.", "Methods Electrolyte Deposition and Fuel Cell Fabrication The μ-SOFCs are fabricated through a typical Si-based micro-machining process as previously reported233.", "A patterned Si3N4/Si with free-standing Si3N4 membrane (150 μm × 150 μm) was fabricated as the substrate for electrolyte deposition.", "BZY electrolyte and the GDC cathodic interlayer were both deposited by an ultra-high vacuum PLD/MBE system (PVD Products, USA) equipped with a 248 nm KrF excimer laser (Lambda Physik, Germany).", "Before the deposition, the chamber was evacuated to ultra-high vacuum of <10−8 Torr and then the free-standing substrates were heated up to desired deposition temperature of 800 °C with a heating rate of 25 °C/min.", "The distance between the target and substrate was kept at 80 mm.", "When the setting deposition temperature was reached, pure oxygen gas was introduced into the chamber to maintain a deposition pressure of 1 mTorr, which would ensure oxygen stoichiometry of the deposited sample.", "Sintered BaZr0.8Y0.2O3−δ pellet target was ablated by a pulsed laser with a fluence of 3.0 J/cm2 at a repetition rate of 10 Hz for 30 minutes to fabricate BZY electrolyte thin film.", "The GDC cathodic interlayer was deposited subsequently by ablating a sintered Ce0.9Gd0.1O1.95−δ for 4 minutes with the same deposition parameters.", "After thin film deposition, samples were cooled down to room temperature with a cooling rate of 25 °C/min.", "After the deposition of BZY electrolyte and GDC interlayer by PLD, the Si3N4 supporting layer was removed by relative ion etching (RIE) with CF4 gas, resulting in a free-standing nanoscale electrolyte.", "Porous platinum thin films are deposited on both sides of the electrolyte via RF sputtering technique with Ar pressure of 30 mTorr at room temperature to achieve porous anode and cathode.", "Thin Film Crystallinity and Morphology Characterization The crystallinity and structural phase of deposited films were analyzed by grazing incidence X-ray diffraction (GIXRD) system equipped with a CuKα X-ray source (PANalytical Empyrean XRD, Netherlands) operating at beam intensity of 40 kV and 40 mA.", "The glancing angle X-ray was incident at an angle of 0.5°.", "Cross-sectional micro-structure of the fuel cell was characterized by field-emission scanning electron microscopy (FESEM, JSM-7600F, JEOL, Ltd., Japan) and transmission electron microscopy (TEM, JEM-2100, JEOL, Ltd., Japan).", "Fuel Cell Performance Characterization Fuel cell performance was tested with a customized test station for the measurement of silicon-based μ-SOFCs.", "The μ-SOFC chip was fixed on a stainless steel chamber with gold gasket for sealing.", "The furnace temperature was elevated to the set testing temperature with a heating rate of 10 °C/min.", "An Au coated tungsten probe, which was connected to a micro-positioner, was put in contact with the porous platinum cathode for current collection.", "Dry hydrogen fuel with a flow rate of 20 sccm was supplied to the anode side, and the cathode side was exposed to the ambient air.", "The fuel cell performance was measured by obtaining the current-voltage polarization curves at temperatures from 350 °C to 425 °C.", "For data collection of both the polarization curves and EIS spectra, a Solartron 1470E potentiostats system and a 1255B Frequency Response Analyzer 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[ "Micro solid oxide fuel cell fabricated on porous stainless steel: a new strategy for enhanced thermal cycling ability Micro solid oxide fuel cell fabricated on porous stainless steel: a new strategy for enhanced thermal cycling ability KimKun Joong1ParkByung Hyun1KimSun Jae1LeeYounki2BaeHongyeul2ChoiGyeong Mana1 1Department of Materials Science and Engineering/Fuel Cell Research Center Pohang University of Science and Technology (POSTECH), 77 Cheongamro, Nam-gu, Pohang, Gyeongbuk 37673, Republic of Korea 2Research Institute of Industrial Science and Technology (RIST) Pohang 790-330, Republic of Korea agmchoi@postech.ac.kr 22443 Miniaturized solid oxide fuel cells (micro-SOFCs) are being extensively studied as a promising alternative to Li batteries for next generation portable power.", "A new micro-SOFC is designed and fabricated which shows enhanced thermal robustness by employing oxide-based thin-film electrode and porous stainless steel (STS) substrate.", "To deposit gas-tight thin-film electrolyte on STS, nano-porous composite oxide is proposed and applied as a new contact layer on STS.", "The micro-SOFC fabricated on composite oxide- STS dual layer substrate shows the peak power density of 560 mW cm−2 at 550 °C and maintains this power density during rapid thermal cycles.", "This cell may be suitable for portable electronic device that requires high power-density and fast thermal cycling.", "Miniaturized solid-oxide fuel cells (micro-SOFCs), designed using thin-film techniques can attain high specific energy (W h kg−1) and energy density (W h L−1) and may partially replace Li batteries in portable devices if fabricated successfully1.", "For practical micro-SOFCs, structural design, substrate and materials of membrane electrode assembly (MEA, or cathode/electrolyte/anode) must be carefully considered12.", "Micro-SOFCs can be of either free-standing membrane (or electrolyte) or supported-membrane type.", "Free-standing membranes are typically fabricated on Si wafers.", "An ultra-thin and dense electrolyte membrane is deposited on an Si wafer and electrodes are deposited on the electrolyte membrane after removing the Si by lithography and etching.", "With well-controlled thin-film MEA of typical geometry, Pt/yttria-stabilized zirconia (YSZ)/Pt cells can achieve power density ≥1 W cm−2 at 500 °C34.", "However, they have extremely short life time, mainly due to instability of nano-porous metal electrodes345 (Table 1).", "In addition, free-standing membranes frequently buckle or fracture during fabrication and operation, so the survival probability of the free-standing membrane upon thermal cycling is poor6.", "These problems may arise due mainly to the low thermal expansion coefficient (TEC) of Si substrate (2.5 ppm K−1) compared with the thin-film MEA (10–20 ppm K−1).", "Thin-film oxide (Gd-doped CeO2) electrode7, tapered Si membrane support8 or metallic grid support5 were introduced to enhance thermomechanical stability of Si-based micro-SOFCs, however thermal cycling ability of free-standing membrane has not been shown to date1.", "More efforts are now being made to increase the stability of cell.", "In this respect, the supported-membrane design is superior because it can provide the mechanical strength required to support the thin-film membrane.", "Various porous materials have been used as substrate for micro-SOFCs91011121314.", "Anodized aluminum oxide (AAO) is an example of a porous substrate9101112.", "The main challenges of this type are that a gas-impermeable electrolyte must be deposited on porous AAO substrate, and that they degrade rapidly due to poor thermal stability of nano-structured AAO and metal electrode.", "Another approach uses currently-available SOFC platforms, e.g., porous cermet anode as a substrate.", "A thin-film anode, electrolyte and cathode on a conventional Ni-YSZ substrate achieved high power density (588 mW cm−2) at 500 °C and good thermal stability (17%/100 h) at 600 °C13, but in this cell, the brittle cermet support can crack upon repeating thermal and redox cycles.", "Fabrication of micro-SOFC on porous metal substrate has been investigated as a way to overcome these problems1516.", "A micro-SOFC supported on porous Ni/stainless steel (STS) dual-layer showed negligible degration of power for 112 h16, but thermal cycling ability of the micro-SOFC with this design was not investigated.", "A nanoporous Ni contact layer with high thermal expansion coefficient (TEC, ~16.5 ppm K−1 at 435 °C) is positioned between YSZ (~10.5 ppm K−1) and STS (~11.5 ppm K−1), so differential expansion and contraction during thermal cyclings may cause fracturing.", "Here, we use an alternative contact layer, La-doped SrTiO3 (LST), due to its TEC comparable to that of the YSZ and STS, high electronic conductivity and redox stability.", "If this material is mixed with YSZ, both good compatibility and nanoporous microstructure can be obtained due to limited sintering or grain growth.", "Thus LST-YSZ composite may be appropriate as a substrate to deposit gas-impermeable thin-film electrolyte.", "Furthermore, the exsolution technique was used to utilize composition of (La, Sr)(Ti, Ni)O3 (LSTN) to improve electrical conductivity and catalytic activity1718.", "Finally, a newly designed dual-layer substrate (LSTN-YSZ/STS) was fabricated by simple co-firing.", "Then a thin-film of oxide-based electrode and electrolyte was deposited in a manner similar to one described previously16.", "To the best of our knowledge, this is the first demonstration of the ability of the thermal robustness of micro-SOFC, which has never been attained in many conventional Si-based devices.", "Experimental procedures The fabrication process is simpler than for other micro-SOFCs because it does not use complicated lithography, etching or templating (Fig. 1, Table 1).", "A dual-layer substrate is prepared using conventional tape-casting (Fig. 1a) and lamination (Fig. 1b).", "Then the green dual-layer is co-fired in reducing gas (Fig. 1c) to avoid oxidation of STS.", "To ensure suitable nanostructure, the dual-layer substrate is characterized after firing.", "The LSTN-YSZ contact layer (thickness ~40 μm) has pore size of ~500 nm and surface root-mean-square roughness (RMS) of 44 nm (Fig. 1c).", "An area porosity ε of LSTN-YSZ surface obtained from binary images, increased from 14 to 18% after surface polishing and a RMS value decreased from ~44 nm to ~21 nm after surface polishing (Supporting Information, Fig.", "S1), thus the porosity and surface roughness are appropriate for deposition of 2-μm-thick and dense electrolyte.", "X-ray diffraction confirmed that LSTN-YSZ on STS after firing exhibited all major peaks of single-phase SrTiO3 and cubic YSZ (Supporting Information, Fig.", "S2).", "A 380-μm-thick STS support has 50-μm particles that are connected to each other well enough to provide mechanical support for the micro-SOFC (Supporting Information, Fig.", "S3).", "The pore size ~10–100 μm and ε ~28% are enough to let fuel gas flow in and reaction by-products (H2O) flow out.", "Further characterization of the dual-layer substrate includes its conductivity as a function of temperature, its area-specific resistance (ASR), and its stability during 100 h at operation temperature and under thermal cycling.", "The electrical conductivity of the dual-layer substrate was measured with temperature (400–550 °C) in wet H2 (97% H2 + 3% H2O) (Supporting Information, Fig.", "S4).", "Due to its metallic conductivity, we assumed that STS does not contribute to the substrate resistance.", "The conductivity of the LSTN-YSZ increased with temperature (Ea ~ 0.39 eV) and was two to three orders of magnitude higher than that of YSZ19 and one order of magnitude lower than that of LSTN20.", "The conductivity of the LSTN-YSZ composite mainly due to that of the high proportion of LSTN (70 wt%) and its percolation though the porous composite.", "The LSTN-YSZ had ASR ~0.02 Ω cm2 after short-term operation (550 °C, 100 h) and fast thermal cycling (40 °C min−1, 150–550 °C); this ASR is smaller than the usual target value of Ohmic ASR (~0.15 Ω cm2).", "The MEA was deposited by pulsed laser deposition (PLD), with NiO-YSZ as the anode, YSZ as the electrolyte and La0.7Sr0.3CoO3-δ (LSC) as the cathode (Fig. 1d), then a current collector (Pt) was sputter deposited (Fig. 1e) to result in a micro-SOFC (Fig. 1f).", "Further details in experimental procedure can be found in Supporting Information.", "Results and Discussion Total area of a cell (Fig. 2a,b) was 78 mm2, and the cathode area was 3 mm2.", "The active area could be enlarged by careful control of surface defects in the LSTN-YSZ contact layer.", "Due to the robust STS support, the cell provides good mechanical stability, ease of handling, and flexibility.", "Thin Ni or STS-supported cells are mechanically flexible without visible cracks on the electrolyte21; therefore, this type of cell may show mechanical stability when stacked vertically, thereby overcoming one of the shortcomings of conventional SOFCs.", "The microstructure of a cell was observed after electrochemical tests.", "A thin-film MEA consists of 0.7-μm-thick LSC, 2-μm-thick YSZ (Fig. 2c) and 0.6-μm-thick Ni-YSZ (Fig. 2d).", "The YSZ electrolyte looks dense and has no pinholes.", "Both electrodes have similar nanostructured grain size or pore size (<100 nm).", "The rough surface of STS was covered by LSTN-YSZ, which has small and uniform pore size (<0.5 μm, Figs 2e and 1c).", "Pore size and surface smoothness of a substrate significantly affect the structural stability and morphology of thin films22.", "In a preliminary study, we used Ni-YSZ as a nano-porous contact layer instead of LSTN-YSZ as similarly shown in the literature2324.", "However, the pore size and porosity of the Ni-YSZ are ~1 μm and 27%, respectively, and both are higher than those of LSTN-YSZ.", "Because Ni particles are easily sintered during co-firing in a reducing atmosphere25; the resulting surface was not appropriate as a target for deposition of 2-μm-thick MEA.", "Cr poisoning during cell firing mostly degrades Ni-YSZ anode and thus it is not quite significant in this study since we have deposited Ni-YSZ on pre-fired substrate.", "However we have analyzed the mutual elemental diffusion between LSTN-YSZ and STS of as-fired (1250 °C) bi-layer substrate.", "There was negligible Fe or Cr diffusion from STS layer into LSTN-YSZ layer.", "Thus LSTN-YSZ can be used as diffusion barrier layer (DBL).", "We have previously confirmed that YST (Y-doped SrTiO3)-CeO2 layer can be used as DBL25.", "Thus, we confirm that a LSTN-YSZ/STS dual-layer fabricated by simple co-firing is a suitable porous substrate to meet microstructural requirements, electrical properties, thermal stability, and chemical stability.", "Current-voltage (I-V) curves of the cell at 450–550 °C show that the open-circuit voltage (OCV) was >1.05 V (Fig. 3a, left y axis).", "This high voltage indicates that the thin-film electrolyte is quite dense without pinholes or cracks, and has a good seal.", "For micro-SOFCs fabricated on porous substrate, a reasonably high OCV value (≈Nernst voltage) is often limited due to large pore size, roughness, and defects of the deposition surface or to electrolyte damage during lithography and etching26.", "However, the substrate used in this study is fabricated without lithography and etching, and the YSZ/Ni-YSZ films are thick enough (≥2 μm) to close the pore openings (~500 nm) of the LSTN-YSZ substrate (Fig. 2e).", "To the best of our knowledge, only one study reported OCV >1 V with 3–5 μm thick YSZ electrolyte which was sputtered on Ni-YSZ/STS substrate23.", "The peak power density (PPD) was 235, 370 and 560 mW cm−2 at 450, 500 and 550 °C (Fig. 3a, right y axis).", "The contributions of Ohmic ASR ASRΩ and polarization ASR ASRp, were extracted from the impedance spectra (IS) of the cell measured under open-circuit condition (Fig. 3b).", "The high-frequency intercept (Fig. 3b, inset) and low-frequency intercept are associated with ASRΩ and ASRP, respectively.", "The ASRΩ value was used to calculate that the ionic conductivity of the 2-μm-thick YSZ film was 9.74 × 10−4 S cm−1 at 500 °C, which is comparable to that of bulk YSZ (1.1 × 10−3 S cm−1) at 500 °C19.", "The IS patterns show that the total ASR ASRtot of the cell is primarily determined by ASRP, which was 97, 96 and 93% of ASRtot at 450, 500, and 550 °C, respectively; this high percentage confirms that the resistance of the cell is limited by ASRP.", "Although further interpretation of limiting factor of reactions pathways for thin-film electrode was not possible at the present study, microstructure and thickness of the films may have important contributions.", "For example, deposition of same thin-film compoment on nano-porous Ni substrate with 6-μm-thick Ni-YSZ, 2-μm-thick YSZ and 6-μm-thick LSC achieved PPD of 110 mW cm−2 at 570 °C14.", "Although indirect, this comparison indicates that microstructure and thickness of thin-film electrode for the present cell may have more reaction sites (TPB) and sufficient gas transport than aforementioned cell.", "The thermal stability of the cell was tested by applying ten thermal cycles between 350–550 °C up to 15 °C min−1 durations at 550 °C for 6 h (Fig. 3c).", "To check thermal robustness of the cell during the test, OCV was monitored in-situ during the entire test time, and IS and Current-voltage-power (I-V-P) curves were measured between each pair of thermal cycles at 550 °C.", "During the first ten thermal cycles, OCV was >1 V; this consistency indicates that cracks were not generated in the YSZ electrolyte.", "The state-of-the-art free-standing micro-SOFC has a huge thermal mismatch between free-standing electrolyte and Si substrate, so thermal cycling may damage the free-standing memebrane.", "Nonetheless, in a recent study, rapid thermal cycling ability of Si-supported cells caused no membrane fracture over several cycles, but specific changes in OCV were not reported so the stability of the YSZ electrolyte has not been established7.", "In contrast, we confirmed negligible OCV degradation under rapid thermal cycles.", "ASR change was also observed during thermal cycling (Fig. 3c, inset); little degradation was observed in either ASRΩ or ASRP.", "Therefore, an initial peak power density was remained at the end of the thermal cycling.", "The stable ASRΩ means that the cell has a stable interface without electrolyte cracks or de-lamination between the cell components, and also has little interfacial reaction.", "The stable ASRP might be utilized to eliminate time-dependent microstructure degradation of thin-film electrode, i.e., densification of nano-porous Pt electrodes, which is a major problem in typical micro-SOFC devices (Pt/YSZ/Pt on Si)345.", "Because we used an oxide-based electrode, the densification of thin-film microstructure was limited.", "A Ni-YSZ thin-film anode requires post-annealing at high temperature (1200 °C) to stabilize its microstructure, because the Ni-YSZ thin-film has a large driving force for Ni coarsening caused by minute equiaxed crystallites (diameter of several nanometers)27.", "However, the Ni-YSZ film used in this study showed little Ni coarsening without annealing at high temperature and operation at 550 °C for 13 h (Fig. 2d); this novel finding will be discussed in future work.", "For LSC thin-film cathodes, chemical compatibility with YSZ at such a low temperature could be a concern because Noh et al. suggests necessity of GDC buffer layer between Co-containing cathode, e.g.", "LSC, and YSZ due to the formation of insulating phase even at the temperature less than 650 °C28.", "We are currently fabricating the cell with GDC buffer layer and the results will be reported.", "Thermal stability of multi-layered devices such as SOFCs is determined primarily by thermal stress between cell components, as a consequence of mismatched TECs.", "However, for small cells (area ~78 mm2) and thin layers (thickness ≤50 μm, excluding STS layer) like the present cell, the cell is resistant to failure caused by cracking or delamination due to the temperature gradient.", "In contrast, a conventional anode-supported cell (ASC), i.e.", "Ni-YSZ supported cell, often cracks after cooling to room temperature although the cell size is small.", "The cracks occur due to TEC mismatch between YSZ electrolyte and the sealants or cell holder (alumina tube).", "The TEC of the commercially-available SOFC sealant used in this study is 12.6 ppm K−1, which is reasonably-matched with that of the main cell structure: YSZ (10.5 ppm K−1), Ni-YSZ (12.5 ppm K−1), LSTN-based layer (11–12 ppm K−1) and STS (11.2 ppm K−1)2930.", "However, the alumina tube has much lower TEC (7.9 ppm K−1) than the cell components; the mismatches in TEC may be the cause of cracking during thermal cycle.", "A 50 μm-thick YSZ electrolyte layer (9-mm diameter), with additional 30 and 40 μm-thick cathode and anode, respectively, supported on a 2 mm-thick YSZ ring by using YSZ paste survived without cracking and thus no severe OCV and ASR degradation after thermal cycles between 200–800 °C (50 °C min−1)31; the authors predicted that 1-cm-thick YSZ with YSZ electrolyte—YSZ ring—YSZ paste configuration can survive up to 200 °C min−1 thermal cycles.", "Thus cracks are induced mostly due to TEC mismatch between YSZ and cell components or sealants.", "Surprisingly, the current cells never crack during fast thermal cycles or even cooling to room temperature.", "We speculate that the porous but ductile STS substrate may absorbed the thermomechanical stress caused by sealants or the alumina tube during thermal cycles.", "This resistance to cracking demonstrates the thermal robustness of micro-SOFC supported by porous STS.", "Among the cell components, the LSC cathode has the highest TEC of 21.3 ppm K−1, so de-lamination of the LSC film from an electrolyte surface may be expected.", "Nonetheless, due to the small area of the cathode (3 mm2), the ASR of the cell was maintained during thermal cycles.", "Among numerous types of micro-SOFCs, successful demonstration of thermal cycling ability has been rare.", "One paper reported a thermal cycling experiment with a micro-SOFC built on conventional Ni-YSZ substrate; the result was quite encouraging13.", "But this cell may also fail during cooling to room temperature due to the brittle nature of Ni-YSZ cermet as a substrate, and its contact with sealants.", "We conducted additional durability test and its result is presented in Supporting Information, Fig.", "S5.", "Fifty thermal cycles were repeated with wide temperature range (150–500 °C) and heating/cooling rates of 20 °C min−1.", "OCVs were measured in-situ during thermal cycles.", "OCV >1 V was maintained throughout the thermal cycles; this consistency indicates that the electrolyte did not crack.", "The results again confirm the thermal cycling stability of the present micro-SOFC.", "Although the tests cannot guarantee the durability of current cell as practical micro-SOFCs, to the best of our knowledge, this is the first demonstration of thermally robust micro-SOFCs fabricated on porous STS substrate.", "A final goal of this research is to fabricate micro-SOFCs that are both durable and produce high power density.", "In micro-SOFCs that use YSZ electrolyte, the relationship between initial peak power density and operation temperature differs among designs (Fig. 4).", "The degradation rate [% h−1] of peak power density was calculated based on the cell test time (Table 1); values range from 4.2–14% h−1 for free-standing Pt/YSZ/Pt on Si345, 1.0–7.5% h−1 for Pt/YSZ/Pt on AAO101112 and 0–0.17% h−1 for LSC/YSZ/Ni-YSZ on Ni-YSZ, Ni and LSTN-YSZ/STS substrates1314.", "A Pt/YSZ/Pt cell supported on Si can achieve high power density at low temperature, but rapid degradation is difficult to avoid, mostly due to instability of the nano-porous Pt electrode.", "A cell supported on AAO has additional instability due to poor thermal stability of AAO.", "Although use of durable ceramic electrodes in free-standing YSZ membranes has been studied, successful demonstration of both thermal cycling ability and durability has been limited7.", "In contrast, the cell with oxide-based electrode supported on porous substrate in this study shows small degradation rate.", "The power density of this cell can be further improved by using alternative compositions of thin-film electrode and electrolyte, and by tailoring its microstructure.", "The realization of micro-SOFC fabricated on porous STS substrate reinforces the feasibility of this technology and may provide a new implementation strategy.", "Long-term tests with a constant electrical load will be conducted for chemical stability, and fuel versatility will be assessed as ultimate studies of the reliability of micro-SOFCs.", "The slow and expensive PLD process will also be replaced by sputtering process which allows faster deposition with larger area.", "Large-size membranes are always favorable when assembling cells to form stack132.", "In summary, the fabrication and thermal robustness of a micro-solid oxide fuel cell (micro-SOFC) was demonstrated.", "An oxide-based thin-film membrane electrode assembly was deposited on top of a dual-layer substrate.", "The substrate consists of porous LSTN-YSZ as a contact layer to deposit gas-tight YSZ thin-film electrolyte on it and STS as a thermo-mechanical support.", "The cell attained peak power density of 560 mW cm−2 at 550 °C with wet H2 fuel gas and maintained this power density during rapid thermal cycling.", "This cell may be suitable as a power source for small portable electronic devices that require high power density and fast thermal cycling.", "The results may help to further advance process science and technology of micro-SOFCs that use thin-film components.", "Additional Information How to cite this article: Kim, K.", "J. et al.", "Micro solid oxide fuel cell fabricated on porous stainless steel: a new strategy for enhanced thermal cycling ability.", "Sci.", "Rep. 6, 22443; doi: 10.1038/srep22443 (2016)." ]

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[ "Tailoring the Microstructure of a Solid Oxide Fuel Cell Anode Support by Calcination and Milling of YSZ Tailoring the Microstructure of a Solid Oxide Fuel Cell Anode Support by Calcination and Milling of YSZ HanifiAmir Reza1Laguna-BerceroMiguel A.a2SandhuNavjot Kaur1EtsellThomas H.1SarkarPartha3 1Department of Chemical & Materials Engineering, University of Alberta, Edmonton, Alberta T6G 1H9, Canada 2Instituto de Ciencia de Materiales de Aragón (ICMA), CSIC- Universidad de Zaragoza, C/Pedro Cerbuna 12, E-50009, Zaragoza, Spain 3Environment & Carbon Management, Alberta Innovates - Technology Futures, Edmonton, Alberta.", "T6N 1E4, Canada amalaguna@unizar.es 27359 In this study, the effects of calcination and milling of 8YSZ (8 mol% yttria stabilized zirconia) used in the nickel-YSZ anode on the performance of anode supported tubular fuel cells were investigated.", "For this purpose, two different types of cells were prepared based on a Ni-YSZ/YSZ/Nd2NiO4+δ-YSZ configuration.", "For the anode preparation, a suspension was prepared by mixing NiO and YSZ in a ratio of 65:35 wt% (Ni:YSZ 50:50 vol.%) with 30 vol.% graphite as the pore former.", "As received Tosoh YSZ or its calcined form (heated at 1500 °C for 3 hours) was used in the anode support as the YSZ source.", "Electrochemical results showed that optimization of the fuel electrode microstructure is essential for the optimal distribution of gas within the support of the cell, especially under electrolysis operation where the performance for an optimized cell (calcined YSZ) was enhanced by a factor of two.", "In comparison with a standard cell (containing as received YSZ), at 1.5 V and 800 °C the measured current density was −1380 mA cm−2 and −690 mA cm−2 for the cells containing calcined and as received YSZ, respectively.", "The present study suggests that the anode porosity for improved cell performance under SOEC is more critical than SOFC mode due to more complex gas diffusion under electrolysis mode where large amount of steam needs to be transfered into the cell.", "Nickel-YSZ is the commonly used anode material in solid oxide fuel cells (SOFCs) due to its high performance at intermediate temperatures.", "The fuel cell anode needs to have a suitable microstructure resulting in high electronic conductivity as well as low activation and concentration polarizations.", "In order to obtain high electrical conductivity, nickel particles need to form a percolative network.", "Nickel also provides high catalytic activity and transfers the electrons from the functional layer to the current collector.", "Sufficient anode porosity is crucial for the fuel gas to diffuse and for the removal of the reaction products.", "However, porosity needs to be optimized without negatively affecting the mechanical strength of the anode12.", "YSZ has several functions in the anode microstructure including providing ionic conductivity, limiting nickel sintering, matching the thermal expansion coefficient of the anode with the electrolyte and broadening the triple phase boundaries (TPBs), where nickel (electronic conductor), YSZ (ionic conductor) and pores (fuel gas channels) meet345.", "Electrochemical performance and durability of the anode is a function of microstructure and thus TPB length.", "Larger TPB length leads to a reduction in polarization4.", "It is believed that a finer microstructure having a uniform distribution of particles and pores increases the TPB length56.", "The effect of nickel particle size and distribution on the overall anode performance has been studied by several researchers where it was found that the anode conductivity is highly affected by the powder synthesis technique and was shown that an anode with finer microstructure provides lower resistance789.", "The Ni-YSZ ratio has also been identified as an important criterion in the extension of the TPBs.", "High nickel or YSZ content has an adverse effect on the TPB length9.", "Wilson et al. identified the highest TPB length when nickel was 34% of the solid volume8.", "Of particular interest is the distribution of channels along the fuel electrode, especially under solid oxide electrolysis cell (SOEC) mode, as high amounts of steam must be transported9.", "Anode porosity has been found to be an important factor in cell microstructure and thus power performance.", "Porosities in the range of 50 vol.% for the anode supported microtubular cells are typically used10.", "Suzuki et al.11 varied the anode porosity in anode supported SOFCs by controlling the sintering temperature and found that the more porous sample (54%) had finer nickel particles and better performance due to the ease of gas diffusion.", "The effect of gas diffusion using infiltrated electrodes was studied in detail by Hussain et al.12.", "They found that the resulting impedance due to gas diffusion in infiltrated electrodes showed a clear dependency on the structural parameters of the electrode.", "The effect of gas diffusion is even more important in electrolysis mode.", "Recently, Ebbesen et al.13 studied this effect in Ni-YSZ anode supported cells with different porosity (28% and 34%).", "They found that changing the porosity of the support structure results in a change in the Ni–YSZ TPB resistance and a significant change in the low frequency concentration related resistance at high current densities.", "They observed increased polarization in EC-mode while decreasing the porosity shows that diffusion limitations cannot be neglected for support structures with porosities below 30% (with a support thickness of 300 μm).", "The effectiveness of using calcined YSZ in the development of a porous structure for infiltration of nickel1415 or LSBT16 anodes as well as LSM1718 or Nd nickelate19 cathodes has been previously shown by the authors.", "Despite many studies on the effect of nickel particle size and content on anode microstructure and thus performance, there is a lack of information in the literature regarding the effect of using processed YSZ in the conventional nickel-YSZ anode on electrochemical performance.", "The aim of the current study is to investigate the influence of using calcined-milled YSZ vs. as received YSZ in the anode microstructure on cell performance under both SOFC and SOEC modes.", "In this manuscript the anode supported fuel cells with as received Tosoh YSZ and calcined YSZ in their Ni-YSZ anode support are referred to as “TY” and “CY”, respectively.", "Results and Discussion Microstructural analysis Figure 1a,b represent the cross-sections of TY and CY following electrochemical testing.", "The thicknesses of the anode supports are about 360 and 500 μm for the TY and CY cells, respectively.", "The interfaces between the entire cathode thickness, electrolyte and part of the anode for the TY and CY cells are shown in Fig. 1c,d, respectively.", "The cathode and the electrolyte shown for both cells have similar thicknesses of about 50 μm and 13 μm, respectively.", "The anode microstructure shows the pores formed due to the burning of the graphite pore-former (slit shaped pores), and smaller pores which correspond to intergranular pores and porosity formed due to the reduction of NiO to Ni.", "It is worth noting that the anode of the TY cell is less porous with finer pores compared with the anode of the CY cell.", "Figure 1e,f shows a suitable distribution of the Nd nickelate cathode (needles or plate like particles) near the interface of the cathode and electrolyte.", "Considering the weight gain of the cathode following infiltration of Nd nicklate, the YSZ:Nd nickelate ratio was calculated to be 69:31 vol.% and a 14% decrease in the total open porosity of the cathode was found leading to a porosity reduction from 50% to 36%.", "Table 1 shows the porosity of the TY and CY anodes before and after reduction.", "Following sintering at 1350 °C, both microstructures have a significant amount of closed pores (see Fig. 2a,c).", "After reduction, the amount of closed porosity in both microstructures decreases and open porosity increases (see Fig. 2b,d).", "The CY anode microstructure remains more porous than the TY anode both before and after reduction.", "The pores caused by the pore former are larger (5–20 μm) than the intergranular pores and the porosity caused by NiO reduction (∼1 μm).", "These finer pores have more impact on the triple phase boundary length than the larger pores formed by graphite.", "However, larger pores provide excellent channels for gas diffusion into the reaction points.", "The comparison of the high magnification images shown in Fig. 2e,f reveals that the less porous TY anode contains finer pores.", "The distribution of the pores (not formed by the graphite pore-former) and their average size in both anodes presented in Table 1 confirms this.", "This might be the reason for its similar surface area (see Table 1) to the CY anode despite the fact that the former anode is less porous.", "It was previously shown by the authors that following 72 hr ball milling of as received Tosoh YSZ, its particle size (250 nm for as received powder and 240 nm following milling) and surface area (13.19 m2/g for as received powder and 12.38 m2/g following milling) remain relatively constant20.", "However, the particle size of 1500 °C calcined YSZ (75 μm) shows a significant decrease following 72 hr ball milling (760 nm) and its surface area after calcining (0.03 m2/g) increases following milling (3.23 m2/g).", "Therefore, the milled-calcined YSZ maintains larger particles and a lower surface area compared with the as received powder.", "The increased particle size of calcined-milled YSZ compared with as received powder is a major reason for the reduced sinterability high porosity and larger pores in the anode microstructures containing calcined powder.", "This is also confirmed by the lower shrinkage rate of this sample following sintering (see Table 1).", "Electrochemical Characterization The electrochemical performance (current density versus voltage curves) for TY and CY cells under fuel cell and electrolysis operation modes can be observed in Fig. 3.", "Initial characterization was performed at 800 °C under pure humidified hydrogen (100 mL/min H2 through a water bubbler kept at room temperature: ~3 vol.% steam content).", "As observed in the figure (black solid and hollow squared symbols), the performance of both TY and CY cells is rather similar under SOFC mode, as current densities of about 600 mA cm−2 were achieved for both cells at 0.7 V.", "However, this value is much higher than that obtained for cells fabricated using the same methodology but using standard LSM-YSZ oxygen electrodes, where current densities in the range of 380 mA cm−2 were measured under identical operating conditions21, and also higher than standard anode supported micro-tubular cells (NiO-YSZ/YSZ/LSM-YSZ)10.", "In addition, comparable values were reported by the authors for similar cells also using Nd nickelate infiltrated into a thin porous YSZ layer as the cathode19.", "EIS spectra recorded under OCV conditions are plotted in Fig. 4, and the fitted parameters, using the LRs(R1/CPE1)(R2/CPE2)(R3/CPE3) equivalent circuit, are summarized in Table 2.", "Although ASR values are reasonably similar for both cells (1.48 Ωcm2 and 1.55 Ωcm2 for the TY and CY cell, respectively), the EIS spectra are rather different.", "As observed in Table 2, Rs is smaller for the CY cell.", "This is consistent with the densification of the YSZ electrolyte, as some porosity is observed for the TY cell (Fig. 1c).", "The co-sintering process of the green tube/electrolyte layer for the TY cell could be further optimized.", "Poor lateral current collection might be also contributing to this increased ohmic resistance for the TY cell.", "In addition, the R1 contribution is in the range of 0.035–0.04 Ωcm2 appearing at frequencies of ∼10–20 kHz.", "As previously observed by different authors, this process is attributed to charge transfer at the oxygen electrode/electrolyte interface2223.", "Furthermore, R1, the high frequency (HF) component, is not changing for both cells, confirming that this contribution is produced by the common Nd nickelate-YSZ oxygen electrode.", "R2, the medium frequency (MF) component, and R3, the low frequency (LF) component, occurring at frequencies of ∼0.1–2 kHz and ∼1–10 Hz, are generally attributed to charge transfer and gas diffusion at the fuel electrode, respectively1024.", "As observed in Table 2, when using the calcined powder (CY cell), the LF component was lower (improved diffusion in the anode support as a consequence of the optimized porosity) whereas the MF component was higher.", "The increase of the MF component is due to lower activation energy which is consistent with the larger pore distribution which affects the TPBs.", "CY has higher activation polarization but lower concentration polarization than TY and this can be the reason for their similar power performance under SOFC mode.", "SOFC-SOEC electrochemical characterization was also performed using a high steam concentration (mixtures of 50% steam–50% hydrogen as fuel) (see Fig. 3).", "Under these conditions, although the performance of both TY and CY cells is rather similar under SOFC mode, concentration polarization is clearly observed at high current densities for the TY cell (above ∼400 mAcm−2 at 700 °C and 800 °C), as a consequence of the non-optimized porosity obstructing an appropriate flux of hydrogen and steam.", "This effect is much more noticeable under electrolysis (SOEC) mode, despite the wall thickness difference of the anode supports (∼360 and ∼500 μm for the TY and CY cells, respectively).", "Much higher current densities were measured for the CY cell as a consequence of the greater number and larger pores at the fuel electrode, especially when increasing the voltage and the operating temperature.", "For example, at 1.5 V and 800 °C, the measured current density for the CY cell was increased by a factor of two in comparison with the TY cell (−1380 mA cm−2 and −690 mA cm−2, respectively).", "The performance of the TY cell is similar to other micro-tubular SOEC cells reported in the literature25.", "From our knowledge, the SOEC performance of the CY cell is the highest reported for micro-tubular electrolysis cells26.", "The current results confirm that the pore content and its size distribution in the CY cell are responsible for the increased performance, in particular for electrolysis applications.", "The effect of gas transport for both cells is illustrated in the EIS experiments performed as a function of the steam content in the fuel electrode (see Fig. 5) under OCV conditions.", "Using low steam contents for the TY cell, the polarization resistance of the cell significantly increases, as a consequence of a gas transport limitation.", "When increasing the steam content, this polarization resistance is reduced.", "However, for the CY sample even for low steam contents, the polarization resistance is approximately constant for the full range studied as a consequence of the optimized porosity.", "Additional information can be obtained from the EIS data generated under current load (Fig. 6).", "Analysis of the impedance spectra for single cells using equivalent circuits is complex, as some of the electrode processes usually overlap, as is the case for the CY cell (Fig. 6b).", "The fitted parameters, using the equivalent circuit previously described, are also summarized in Table 2.", "It is important to note that these experiments were performed using moderate current loads (±200 mA) due to limitations of the equipment.", "As observed in the inset of Fig. 3, at those current densities, the TY cell outperforms the CY cell, as in this region of the j-V curve activation polarization is more dominant than concentration polarization.", "In any case, these experiments confirmed that the HF contribution corresponds to the Nd2NiO4+δ-YSZ oxygen electrode as it remained almost constant for all the conditions studied in both cells.", "The most significant change is the decrease of the LF contribution for the CY cell under negative polarization (SOEC conditions), as a consequence of the optimized gas diffusion within the Ni-YSZ support.", "Positive impacts of using calcined YSZ in developing a porous YSZ microstructure for conversion to an anode or cathode upon infiltration has been previously shown by the authors1415161819212728.", "When cell infiltration for the purpose of improving the catalytic activity or the electronic/ionic conductivity (or both) of the anode is planned, an anode with larger pore size and higher porosity (~50%) than TY is desirable (due to pore clogging during infiltration).", "CY can offer the potential microstructure very effectively.", "It is also noticeable that the initial particle size of both calcined YSZ and NiO following 72 h ball milling is submicron for which, according to Yu et al.29, the resulting anode cermet has a fine microstructure of well percolating phases which provides suitable electrical and mechanical properties.", "They have shown that very large particles of NiO and YSZ have negative effects on both the electrical and mechanical properties of the anode cermet.", "Conclusions From the comparison of the anodes containing as received Tosoh YSZ or calcined YSZ, the following conclusions can be drawn: The anode containing as received Tosoh YSZ had less porosity (33%) compared with the anode containing calcined-milled YSZ (46%).", "This negatively affects the gas diffusion in the first anode especially under SOEC mode.", "In the case of the anode containing as received Tosoh YSZ, the pores located in the anode functional layer contributing to the triple phase boundaries are finer which can lead to an increase in TPB length and reduction of the cell activation polarization.", "The anode containing calcined YSZ shows sufficient porosity for infiltration thereby enhancing its electrochemical performance while the anode containing Ni-Tosoh YSZ can have blocked pores following infiltration.", "Electrochemical performance in SOFC mode is similar for the as received Tosoh YSZ and the calcined YSZ cell.", "For the calcined cell, gas diffusion improved while activation polarization deteriorated.", "These contributions compensated each other.", "Gas diffusion plays a crucial role in electrolysis mode.", "An optimized microstructure of the anode support led to an increase by a factor of two of the current density at 800 °C and 1.5 V.", "Methods Cell Fabrication The anode supported cells studied in this paper were fabricated by slip casting of a NiO-YSZ anode support followed by dip coating of a thin YSZ electrolyte and a thin porous YSZ layer for cathode infiltration.", "Nd2NiO4+δ was infiltrated into the thin porous YSZ layer of both cells to form the cathode.", "In order to prepare a suitable slip for casting the anode supported cells, as received YSZ (TZ-8Y, 8 mol% Y2O3, Tosoh) or its calcined form (calcined at 1500 °C for 3 h) was mixed with 65 wt% NiO powder (Baker Chemicals, <3 μm) and water at a powder:water weight ratio of 1:1.", "The mixture was then milled at 120 rpm for 72 h in a plastic bottle with 5 mm zirconia balls.", "Additional water was added after milling to adjust the solid loading of the final suspension to 40%.", "The pH of the slip was set to 4.0 using 2% hydrochloric acid.", "In order to generate high porosity, 30 vol.% graphite (Sigma Aldrich <325 mesh) was incorporated into the slip following pH adjustment, and then the suspension was mixed for 15 minutes prior to slip casting.", "To create the tubular support, the slip was cast into a plaster mold (previously prepared from a tubular mandrel) and left for about 1 minute, after which the excess slip was quickly poured out.", "Several pellets (15 mm diameter, 5 mm thick) were also slip cast in a plaster mold using the same slip.", "The wet tube and pellets were then dried at room temperature for 1 h.", "The resulting drying shrinkage facilitates removal of the green bodies.", "The green tube was dried at 100 °C, heated at 700 °C for 1 h to oxidize all the graphite, and then pre-sintered under air at 1100 °C for 3 h.", "The slip cast pellets were also sintered under a similar sintering regime except their final sintering temperature was 1350 °C.", "The electrolyte and the thin porous YSZ layer formulae and their dip coating procedure are explained elsewhere141528.", "Both layers were sintered at 1350 °C for 3 h.", "Infiltration of Nd2NiO4+δ into the thin porous YSZ layer has also been addressed19.", "Density and porosity measurements were carried out on the slip cast and sintered pellets using Archimedes principle.", "The same pellets were used for calculation of the sintering shrinkage.", "Characterization Krypton adsorption/desorption isotherms at 77°K and surface area measurements on the reduced anode pellets were performed by Quantachrome Autosorb-1.", "Scanning electron microscopy (SEM) was carried out on the fuel cells and anode pellets using a Zeiss EVO LS15 EP-SEM instrument.", "The pore size of the reduced anode samples was measured by SEM image analysis.", "Electrochemical measurements Electrochemical studies were performed in the temperature range between 600 °C and 800 °C in both fuel cell and electrolysis modes using a similar experimental setup as previously described181921.", "A fuel composition of 97% H2–3% H2O was used for operation in fuel cell mode, and 50% H2O–50% H2 was used for operation in reversible mode.", "For the inner contact (hydrogen electrode), silver wires were welded onto silver mesh and mechanically pressed inside the micro-tubes (6mm inner diameter, 60 mm long).", "Silver paste was also added to the mesh to improve contact.", "For the outer contact (oxygen electrode), a thin gold layer was added by dip coating and, subsequently, a gold wire was coiled around the cathode surface (1 cm2) and Au paste was added to improve electrical contact and current collection.", "The cells were then sealed to an alumina tube using an alumina-based ceramic sealant (Aremco, Ceramabond 503) and heated to 800 °C under nitrogen, while the oxygen electrode side was exposed to ambient air.", "Subsequently, nitrogen gas was switched to pure humidified hydrogen, reducing NiO to metallic Ni at the anode.", "Steam was supplied by the use of a direct vapour humidifier controlling the relative humidity with a resolution of ±1.3%.", "All gas lines located downstream of the humidifier were externally heated in order to prevent steam condensation. j-V (current density-voltage) was recorded in galvanodynamic mode using a scan rate of 2.5 mA cm–2 s–1.", "EIS (electrochemical impedance spectroscopy) measurements were performed under OCV (open circuit voltage) conditions and also under current load (±200 mA), using 20 mV of sinusoidal amplitude and a frequency range from 100 kHz to 100 mHz.", "These experiments were performed using a VSP potentiostat/galvanostat (Princeton Applied Research, Oak Ridge, USA).", "Additional Information How to cite this article: Hanifi, A.", "R. et al.", "Tailoring the Microstructure of a Solid Oxide Fuel Cell Anode Support by Calcination and Milling of YSZ.", "Sci.", "Rep. 6, 27359; doi: 10.1038/srep27359 (2016).", "The authors would like to acknowledge the Climate Change and Emissions Management Corporation (CCEMC) of Canada and Fundacion Domingo Martinez and Ministerio de Economia y Competitividad (grant no.", "MAT2015-68078-R) of Spain for funding this research.", "MinhN.", "Q.", "Ceramic fuel-cells.", "J.", "Amer.", "Ceram.", "Soc. 76, 563–588 (1993).", "PratiharS.", "K., DassharmaA. & MaitiH.", "S.", "Processing microstructure property correlation of porous Ni-YSZ cermets anode for SOFC application.", "Mater.", "Res.", "Bull. 40, 1936–1944 (2005).", "AtkinsonA. .", "Advanced anodes for high-temperature fuel cells.", "Nat.", 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[ "Electrochemical properties of La0.6Sr0.4CoO3 − δ thin films investigated by complementary impedance spectroscopy and isotope exchange depth profiling☆ Electrochemical properties of La0.6Sr0.4CoO3 − δ thin films investigated by complementary impedance spectroscopy and isotope exchange depth profiling☆ KubicekMarkusaHuberTobias M.aWelzlAndreasaPennAlexanderabRuppGhislain M.aBernardiJohannesbStöger-PollachMichaelbHutterHerbertaFleigJürgena aInstitute of Chemical Technologies and Analytics, Vienna University of Technology, Getreidemarkt 9, A-1060 Vienna, Austria bUniversity Service Center for Transmission Electron Microscopy, Vienna University of Technology, Wiedner Hauptstr. 8–10, A-1040 Vienna, Austria The oxygen exchange and diffusion properties of La0.6Sr0.4CoO3 − δ thin films on yttria stabilized zirconia were analyzed by impedance spectroscopy and 18O tracer experiments.", "The investigations were performed on the same thin film samples and at the same temperature (400 °C) in order to get complementary information by the two methods.", "Electrochemical impedance spectroscopy can reveal resistive and capacitive contributions of such systems, but an exact interpretation of the spectra of complex oxide electrodes is often difficult from impedance data alone.", "It is shown that additional isotope exchange depth profiling can significantly help interpreting impedance spectra by giving reliable information on the individual contribution and exact location of resistances (surface, electrode bulk, interface).", "The measurements also allowed quantitative comparison of electrode polarization resistances obtained by different methods.", "Highlights • Complementary investigation by impedance spectroscopy and isotope exchange. • Investigation of the same mixed conducting thin film at the same T with both methods. • Quantitative comparison of resistive contributions. • Discussion on interpretation of impedance data with different equivalent circuits.", "Keywords Mixed conductor Impedance spectroscopy Isotope exchange Surface exchange Diffusion ToF-SIMS Introduction Mixed ionic and electronic conducting (MIEC) oxides are promising materials for electrochemical devices based on gas–solid interactions such as solid oxide fuel cells (SOFCs), gas sensors, or permeation membranes [1], [2], [3], [4].", "Several analytical methods exist to investigate the catalytic activity of MIEC electrodes towards the oxygen reduction reaction (ORR) with two of the most important approaches being electrochemical impedance spectroscopy (EIS) and 18O isotope exchange depth profiling (IEDP).", "EIS yields information on resistive and capacitive contributions of MIEC electrodes on ionic conducting substrates.", "Many properties such as the catalytic activity of surfaces, oxygen non-stoichiometry, chemical diffusion, conductivities, transport reactions across solid|solid phase boundaries, or the formation of impurity phases can thus be indirectly probed.", "However, the correct interpretation of impedance spectra is crucial for the validity of the extracted parameters.", "This interpretation can be trivial for simple spectra [5], [6] but in complex systems impedance analysis is often very difficult and far from being unambiguous.", "An equivalent circuit for mixed conductors was introduced in Ref. [7], but it is also restricted in its applicability, cf.", "Ref. [8].", "Compared to EIS, oxygen isotope exchange and subsequent depth profiling [9] has the simpler methodology for data interpretation even though the experiment itself is more elaborate.", "There, the properties of oxygen exchange are tested by providing an isotopic tracer (e.g. 18O) via the gas phase and establishing a time dependent concentration depth profile in a sample.", "The local tracer concentration is determined by secondary ion mass spectrometry (SIMS) and from the resulting depth profile, ion exchange and diffusion related parameters can be extracted.", "While impedance spectroscopy is a quite common method to investigate mixed conducting thin film electrodes, [6], [10], [11], [12] oxygen tracer experiments are often performed on bulk samples [13], [14], [15], [16].", "Recently, several IEDP measurements of mixed conducting cathode materials were published with the oxide films being deposited on insulating substrates [17], [18], [19].", "However, to the best of the authors' knowledge no study so far reported experiments with both techniques being applied on the same films at the same temperature.", "This contribution reports the results of a study applying EIS and IEDP to one and the same La0.6Sr0.4CoO3 − δ (LSC) thin film in order to get complementary results on the resistive contributions of the oxygen reduction kinetics on such films.", "As electrical measurements require an oxygen ion conductor, yttria stabilized zirconia (YSZ) was used as substrate for LSC films with two different grain sizes.", "Quantitative material parameters are deduced from both types of experiments and comparison of the data allowed testing the appropriateness of analysis models.", "Experimental LSC powder was prepared via the nitrate/citrate (Pechini) route.", "The following high purity base materials were used: Co 99.995%, SrCO3 99.995%, La2O3 99.999%, HNO3 70% in H2O, 99.999% purity, citric acid monohydrate 99.9998% (all Sigma–Aldrich).", "Pulsed laser deposition (PLD) target was produced by isostatic pressing (5.2 kbar, 2 min) and sintering (1150 °C, 12 h).", "Dense La0.6Sr0.4CoO3 − δ thin films with 200 nm thickness were prepared on 10 × 10 × 0.5 mm3 YSZ (100) single crystals by pulsed laser deposition (PLD).", "A target to substrate distance of 7.0 cm was chosen and the depositions were performed under 0.04 mbar O2, at 400 mJ/pulse laser energy, 10 Hz pulse frequency, and 27 min deposition time.", "Two different substrate temperatures during film growth, measured with a pyrometer (Heitronics KT-19.99), were used to prepare thin films with different grain size denoted LSC-LT (450 °C) and LSC-HT (600 °C).", "Phase purity of the PLD target was investigated by X-ray diffraction (XRD) in Bragg–Brentano geometry (X'Pert PRO diffractometer PW 3050/60, PANalytical).", "For thin films, XRD measurements were performed in parallel beam geometry on a D8-Discover instrument (Bruker AXS) which was equipped with a General Area Detection Diffraction System (GADDS).", "Information along the theta axis and the chi axis (tilted grains) could be obtained at the same time.", "Nanostructure, and grain sizes of both types of thin films were investigated by transmission electron microscopy (TEM) imaging of thin film cross-sections (FEI TECNAI F20).", "Before isotope exchange and electrical measurements, LSC thin films were microstructured by photolithography in order to prepare circular microelectrodes with 200 μm diameter.", "Oxygen isotope exchange experiments were performed by heating to 400 °C in air (12 K/min), changing the atmosphere to 200 mbar 97.1% 18O isotope enriched oxygen (Campro Scientific) for 5 min, and then cooling to room temperature with 60 K/min to freeze the tracer diffusion profile.", "A pre-annealing in oxygen as often reported in literature was avoided for two reasons.", "One reason is that, due to the 18O concentrations above the natural abundance in bottled oxygen [20] a tracer profile would already be created in the sample before the actual tracer exchange experiment.", "The even more important reason is that due to the short diffusion times of ~ 5 min an experimental procedure of: pre-annealing – cooling – gas exchange – heating – annealing would cause a significant contribution to the tracer profiles from the heating step.", "Gas exchange with evacuation at annealing temperature (the procedure used) annihilates any pre-annealing effect due to the very fast chemical diffusion in LSC (few s) at the annealing temperatures.", "By the procedure used, a tracer profile containing chemical and tracer incorporation/diffusion is created.", "However for the used experimental setup, the influence of chemical tracer incorporation in the experiments is negligibly small due to the orders of magnitude higher amount of 18O incorporated by tracer exchange as also explained in more detail in Ref. [17].", "The resulting isotope diffusion profiles were subsequently measured by depth profiling with ToF-SIMS (TOF.SIMS 5, ION-TOF). 25 kV Bi+ primary ions were used in CBA measurement mode.[21] Negative secondary ions were analyzed in areas of 100 × 100 μm2 using a raster of 512 × 512 measured points.", "For depth-profiling, 2 kV Cs+ ions (500 × 500 μm2, ca. 105 nA) were used for sequential ablation of the surface between measuring mass spectra.", "For charge compensation, a low energy electron flood gun (10 V) was employed.", "Following the SIMS measurements, the same thin films (though different microelectrodes) were investigated by impedance spectroscopy.", "Here, 200 μm microelectrodes were contacted by gold covered steel needles (EGON 0.4, Pierenkemper) and measured with an Alpha-A high performance frequency analyzer (Novocontrol, Germany) versus a macroscopic LSC counter electrode at 400 °C in air.", "AC frequencies of 1 MHz to 0.07 Hz with 10 mV effective amplitude were applied to obtain impedance spectra.", "More details on such microelectrode measurements can be found in Ref. [11].", "Results Thin film characterization Thin films were investigated by XRD using theta-2theta and chi-scans.", "For both LSC-LT and LSC-HT no impurity phases were found and all reflexes could be attributed to pseudo-cubic perovskite phase.", "Lattice parameters of the thin films were analyzed from the maxima position of 4 strong reflexes each and the values of a = 0.3826 ± 0.0006 nm for LSC-LT and a = 0.3830 ± 0.0003 nm for LSC-HT were calculated.", "TEM cross section imaging of the two film types as shown in Fig. 1 was performed in order to analyze their nanostructure and grain size.", "Both LSC film types are dense and columnar growth is observed which is expected for PLD grown films on YSZ with the parameters as used.[22] Differences between the two film types are a result of the different deposition temperature, and the obvious difference in grain size was investigated in more detail.", "About 20 cross section images, similar to those shown in Fig. 1 were recorded, and the number of grain boundaries was analyzed in different depths of the film.", "Thus, the average cross-section column thickness was calculated from a representative total cross section length of more than 12 μm each for LSC-LT and LSC-HT films as shown in Fig. 2.", "LSC-HT has the larger grain size throughout the whole film thickness compared to LSC-LT.", "The largest average distance between grain boundaries is present close to the surface with ~ 64 nm for LSC-HT and ~ 33 nm for LSC-LT.", "Close to the LSC|YSZ interface both thin films have the highest grain boundary density and the smallest grains with an average distance of ~ 24 nm (LSC-HT) and ~ 13 nm (LSC-LT).", "Electrochemical impedance spectroscopy In Fig. 3 impedance spectra are shown, measured on circular 200 μm microelectrodes of the differently prepared LSC thin films.", "Several features are visible in both spectra.", "At the highest frequencies a part of a semicircle is visible which can be attributed to the ionic spreading resistance of YSZ underneath the microelectrode.", "The resistance depends on the size of the microelectrode and is inversely proportional to the ionic conductivity of YSZ.", "From this relation and reference measurements of the temperature dependent ionic conductivity of YSZ single crystals it is possible to calculate an average temperature of the microelectrode as discussed in Ref. [11].", "In our measurements the set temperature of the furnace was chosen such that the YSZ spreading resistance corresponded to a temperature of 400 ± 1 °C.", "At lower frequencies the impedance contributions of the electrode become visible.", "A Warburg-like shape of the electrode contribution with almost a 45° straight line is found at medium frequencies, followed by a semicircle-like part at low frequencies.", "Even though these general features are similar for LSC-LT and LSC-HT, also some differences can be observed between their impedance spectra.", "Most obvious, the total electrode resistance is smaller for LSC-LT.", "Differences of the shape are visible in the intermediate frequency part shown in the inset in Fig. 3.", "LSC-HT approaches the 45° range from larger phase angles (semicircle like) while LSC-LT exhibits a very flat spectrum part above ca. 100 Hz.", "Impedance contributions in this intermediate frequency range are often attributed to the electrode|electrolyte interface.[6] Isotope exchange depth profiling In Fig. 4 the oxygen isotope depth profiles are shown, measured by ToF-SIMS on the same samples after annealing in 18O enriched atmosphere at 400 °C for 5 min.", "The isotope fractions c are calculated according to (1) c = counts O 18 counts O 16 + counts O 18 .", "Both depth profiles exhibit a surface isotope fraction of about 10% followed by a drop in concentration in the LSC thin film which can be attributed to the limited ionic conductivity of LSC.", "Then, at 200 nm depth, a transition to a very flat profile in YSZ follows which reflects the high ionic conductivity there.", "Several differences can be observed between the profiles.", "The total amount of incorporated 18O is higher in LSC-LT, the slope of the concentration decay in LSC is different, and a small step in concentration at the interface is observed for LSC-HT and not for LSC-LT.", "The general tendency of LSC-LT having the lower polarization resistance in EIS and showing the higher exchange rate of tracer is therefore matching well, but for an exact analysis and comparison of oxygen transport parameters and resistance contributions, fitting methods are necessary to analyze both sets of data.", "Data analysis Impedance spectroscopy Generalized equivalent circuits for mass and charge transport in mixed conducting systems are extensively discussed by Jamnik and Maier.[7] The equivalent circuits shown in Figs. 5a,b are slightly adapted from Ref. [7].", "The transmission line model in Fig. 5b represents a mixed conducting electrode with surface related resistance Rs, ionic transport resistance Rdiff (here a sum of 50 equivalent resistances RTL in a transmission line) and interfacial resistance Rif.", "A reduced model for surface controlled oxygen exchange and negligible Rdiff is shown in Fig. 5a.", "The capacitors, Cs, Cif and Cdiff = 50 CTL represent the capacitances of surface, interface, and the chemical bulk capacitance (in a transmission line), respectively.", "Q is a constant phase element with the impedance: (2) Z Q = 1 iω n P .For n = 1, Q is equivalent to a capacitor with capacitance P.", "By using Q instead of C in RC elements (sometimes called “Cole Element”) it is possible to model slightly depressed semicircles, which are regularly observed due to non-idealities in samples.", "The model shown in Fig. 5c is an incomplete equivalent circuit which was used to fit only the low frequency part of the impedance spectra.", "In this case, the spreading resistance of the electrolyte RYSZ was determined beforehand from the axis intercept of the high frequency arc and fixed.", "Then only low frequency points, i.e. the main part of the large semicircle, were used for fitting (LSC-HT: 8 Points 1–0.1 Hz, LSC-LT: 7 Points 0.6–0.07 Hz.", "This arc was attributed to the electrode surface reaction in accordance with studies demonstrating a clear correlation of low frequency arc and surface oxygen exchange.[5], [23] The additional resistance value of the electrode Rif+diff includes all other contributions to the total electrode resistance (e.g.", "Rif, Rdiff).", "The results of fitting the impedance spectra with these different equivalent circuits are shown in Figs. 6a,b,c.", "The fits using the reduced circuit (Fig. 5a) could often be applied in literature [24] to quantify spectra of similar electrode materials at higher temperature.", "Here, however, the corresponding model is not suited well to fit the impedance spectra, see Fig. 5a.", "The fits give a larger resistance Rs for the electrode surface and a smaller resistance Rif for the LSC|YSZ interface, but neither the high frequency part nor the low frequency part is well reproduced even though constant phase elements are used (a (Q)).", "As in this model the oxygen diffusion resistance in LSC is neglected, the failure to reproduce the spectra gives evidence that diffusion (also indicated by the 45° angle in Nyquist plot) may indeed contribute significantly to the total electrode resistance.", "Fitting with the equivalent circuit in Fig. 5b, which includes ion diffusion in a transmission line of 50 identical elements, reproduces the measured impedance spectra very well (cf.", "Fig. 6b).", "The fitting parameters of this model suggest a very small interface resistance and a small surface resistance.", "The major part of the electrode resistance is there explained by the resistances in the transmission line which depend on the ionic conductivity of LSC.", "This distribution of resistances would suggest that the rate limiting step of the overall oxygen reduction in these LSC films is chemical bulk diffusion.", "By using the fitting model with only one RQ element in Fig. 5c, the low frequency part of the impedance spectrum is also well reproduced with a single slightly depressed semicircle (n ~ 0.96).", "Assigning this resistance to the electrode surface leaves only a minor part of the total electrode resistance to the contributions of diffusion and the LSC|YSZ interface.", "In this model, the surface exchange of oxygen would be rate limiting, in contrast to the interpretation derived from the fit in Fig. 6b.", "This discussion reveals that an unambiguous conclusion what is the rate limiting step is hardly possible based on these impedance data alone.", "Isotope exchange depth profiling Owing to the diffusion in two phases (LSC, YSZ) an analytical solution for analyzing the measured tracer profiles is not available.", "COMSOL finite elements software was therefore used to numerically solve the diffusion problem with boundary conditions c = 0.971 in the gas atmosphere (18O concentration in the gas) and c = 0.00205 (natural abundance of 18O) in the LSC layer as well as in YSZ before tracer diffusion takes place.", "Two different models were used to numerically analyze the oxygen isotope depth profiles in Fig. 4.", "The simpler model consists of three parameters, k*, D*LSC and D*YSZ.", "The value of D*YSZ was fixed at 1.2 × 10− 10 cm2/s in accordance with conductivity measurements, and only k* and D*LSC were varied to fit the measured depth profiles.", "This model could not exactly reproduce the experimental results (see Figs. 7a,b).", "Particularly the profile in LSC-HT shows significant deviations from the fit result.", "Spatially varying diffusion coefficients in LSC were therefore allowed in a second model.", "For LSC-HT this included three larger zones in LSC with different D* values and a short zone (10 nm) directly at the LSC|YSZ interface.", "The latter represents an interface resistance.", "The LSC-LT films were analyzed in terms of two zones of different D* without an interface region due to absence of a sharp drop there (cf.", "Fig. 4).", "With this second model better matching fits of the isotope depth profiles were achieved and parameters for surface exchange and diffusion could be extracted, see Figs. 7c,d.", "From the fit parameters of both models it is possible to calculate resistive contributions by using the Nernst–Einstein relation.", "In Eq. 3, this is exemplarily shown for the surface exchange coefficient [6], [25], [26]. (3) R s = k B T 4 e 2 k q c 0 Here, kq is the electrical surface exchange coefficient, kB is Boltzmann's constant, T the temperature, e the elementary charge and c0 the total concentration of lattice oxygen (8.90 × 10− 2 mol/cm3 LSC-LT, 8.87 × 10− 2 mol/cm3 LSC-HT) calculated from X-ray diffraction data of the La0.6Sr0.4CoO3 − δ thin films and neglecting oxygen non-stoichiometry.", "An error in the range of ~ 1% (δ ~ 0.03 [27], [28], [29]) can be expected which is not large compared to the necessary simplifications and experimental errors.", "An analogous calculation is possible for the diffusion parameters using Dq/thickness instead of kq.", "As for this calculation the electrical parameters kq and Dq are required, and in the isotope exchange experiment only the tracer parameters k* and D* can be determined, a correction factor is necessary to consider their different values [25] (Eq. 4).", "For the diffusion coefficients this factor is the Haven ratio H and we therefore obtain (4) D q ⋅ H = D ⁎ .In perovskite-type oxides H is often assumed to be very close to the correlation factor of 0.69 [30]; this value is also used in the following.", "The correlation factor of surface exchange (fs) depends on the exact elementary mechanism.", "As a first approximation the same ratio as for diffusion was used according to (5) k q ⋅ f s = k ⁎ , f s ≈ H .", "Even though the quality of the fit is better when using different diffusion coefficients, the extracted values of the resistive contributions are very similar for the two models.", "In both LSC thin films the largest resistive contribution can be attributed to the electrode surface (~ 160 Ωcm2 and ~ 310 Ωcm2 for LSC-LT and LSC-HT, respectively).", "This dominance of the surface resistance is also in accordance with literature results for LSC investigated by impedance spectroscopy at higher temperatures.[24] Transforming the interfacial concentration drop in LSC-HT into an LSC|YSZ interface resistance shows that it amounts only to a very small fraction of the total electrode resistance (~ 3 Ωcm2).", "Larger than this interface resistance, but still smaller than the dominating surface resistance, is the ionic diffusion resistance of LSC.", "Interestingly, significant changes of the diffusion coefficient with depth were extracted for LSC-HT.", "Here, closer to the interface more than a factor of 2 faster diffusion than close to the surface was found.", "For LSC-LT only slight inhomogeneities of the diffusion coefficient were obtained, and here diffusion was faster closer to the surface.", "The reasons for these inhomogeneities as well as for the differences between the LSC-LT and LSC-HT films are most probably caused by the nanostructure.", "A possible difference of oxide ion conduction in LSC grains and grain boundaries may play a role here which leads to changes in depth due to the changing grain boundary density as shown in Fig. 2.", "The increased average diffusion coefficient closer to the interface as observed for LSC-HT would suggest faster diffusion of oxide ions in or along grain boundaries than in the bulk.", "There is some arbitrarity in defining number and size of regions with different diffusion coefficients in Fig. 7, but essential in our context are primarily the total resistances of diffusion and the fact that measurable inhomogeneities exist at all.", "Comparison of the extracted parameters from EIS and IEDP In Table 1, Table 2 the resistive parameters extracted with the different measurement and fitting methods are compared for LSC-LT and LSC-HT.", "When comparing the total electrode resistance RLSCtotal, a systematic difference can be noted between the values from impedance measurements and isotope exchange, showing higher resistance values in the tracer studies.", "The difference of about 30–50% can have several causes.", "The true correction factor between k* and kq is unknown and the chosen value fs = 0.69 for k can be the reason for discrepancies between the resistances obtained by the different methods.", "For a lower factor fs = 0.5 in Eq. 5 the total resistances would fit very well to the values determined with EIS.", "Another possible source for a systematic deviation is the temperature.", "In microelectrode measurements a temperature gradient in the sample is caused by the contact tip.", "Even if the temperature is corrected by the YSZ spreading resistance, a temperature distribution over the electrode area is present that can affect the effective electrode temperature.[31] For typical temperature dependencies of LSC electrode resistances (Ea 1.3–1.6 eV [15], [24]) a 30% change of the total resistance is already caused by a temperature difference of less than 10 °C.", "Accordingly, the still rather similar resistance values obtained by the two techniques are regarded as indication that indeed both methods probe the same electrochemical processes and are appropriate for analyzing the oxygen reduction kinetics of mixed conducting electrodes.", "Fit results of the impedance data show that the total resistances of the EIS models with the transmission line (Fig. 6b) and with only one RQ element (Fig. 6c) are matching well, but the distribution of the resistances to the individual processes is very different.", "Comparing this to the data extracted from 18O experiments we find the simple model c, fitting only one semicircle for the surface resistance, is matching much better.", "This becomes obvious from the ratio of the surface resistance to the other electrode resistances shown in the last row of Tables 1,2.", "Here model c (Fig. 5c) yields values of 5–6, matching best to the values of 6–7 found in tracer experiments.", "The model including the full transmission line finds completely different ratios of about 0.2 here.", "One might get the impression that the model with the transmission line is simply over-parameterized and it should be possible to shift the predominant resistance from Rdiff to Rs while remaining a good fit quality.", "This assumption was investigated by fixing the surface resistance to higher values up to the resistance found by model c.", "However, in these cases the quality of the fit was much lower, and performing a linear least square fit with such starting parameters again yielded fit results with dominating Rdiff.", "From such a quantitative comparison it is also concluded that the more semicircle-like intermediate frequency part of LSC-HT (Fig. 3) can be attributed to existence of a small interfacial resistance Rif of LSC-HT and finds its counterpart in the concentration step of the tracer profile (cf.", "Fig. 7d).", "Concentration step as well as semicircle-like feature at these frequencies are absent for LSC-LT.", "This discussion shows that the apparently exact model b fails to correctly analyze the impedance data.", "It should be kept in mind however, that also model b is based on assumptions, e.g. spatially homogeneous RTL values (constant ionic conductivity) while the profiles of the tracer diffusion experiments strongly suggest that this is not fulfilled here.", "Further, also the chemical capacitance could accordingly vary strongly with depth.", "Both of these inhomogeneities with depth can result from the nanostructure of PLD grown LSC thin films and the change of grain size and grain boundary density with depth as shown in Fig. 2.", "This shortcoming of model b could lead to the wrong material parameters resulting from the fit procedure.", "Accordingly, a misinterpretation of the oxygen reduction kinetics and identification of an erroneous rate limiting step may easily happen when only relying on impedance data.", "Combining two independent and complementary measurement methods in order to investigate the electrochemical properties of mixed conducting electrodes is clearly advantageous.", "Conclusions Impedance spectroscopy and isotope exchange depth profiling were used to investigate the oxygen exchange and transport properties of LSC thin film electrodes on YSZ single crystals.", "Two types of LSC thin films (LSC-LT and LSC-HT, prepared at different temperatures) were considered.", "The same films were consecutively analyzed by the two methods yielding complementary information.", "The choice of the correct equivalent circuit for fitting of the impedance spectra and for separating the total electrode resistance into its different contributions proved to be intricate.", "Different fit models suggested different processes to be rate limiting (surface exchange, diffusion).", "However, in oxygen tracer experiments, it could be unambiguously shown that the oxygen exchange at the surface is rate limiting and the best suited model for impedance analysis could thus be identified.", "Data analysis also allowed a quantitative comparison of the resistances of the electrode surface, of diffusion in the electrode and of oxygen transport across the LSC|YSZ interface extracted by impedance and tracer measurements.", "Only rather small differences of the calculated total electrode resistances were observed between the two methods.", "Further, relative importance of surface exchange and diffusion correspond well in both types of experiments and a small impedance contribution of the LSC|YSZ interface resistance found only for LSC-HT in tracer experiments is well matching to differences in the impedance response of LSC-LT and LSC-HT.", "This shows that analysis of data from impedance spectroscopy can be significantly improved by complementary IEDP experiments especially when spatial inhomogeneities such as different grain sizes with depth are present.", "IEDP gives reliable information on the localization of resistances (surface, electrode bulk, interface) or inhomogeneities of diffusion in depth." ]

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[ "A perovskite oxide with high conductivities in both air and reducing atmosphere for use as electrode for solid oxide fuel cells A perovskite oxide with high conductivities in both air and reducing atmosphere for use as electrode for solid oxide fuel cells LanRong1CowinPeter I.2SengodanSivaprakash1TaoShanwena13 1School of Engineering, University of Warwick, Coventry CV4 7AL, UK 2Department of Chemical and Process Engineering, University of Strathclyde, Glasgow G1 1XJ, UK 3Department of Chemical Engineering, Monash University, Clayton, Victoria 3800, Australia aS.Tao.1@warwick.ac.uk 31839 Electrode materials which exhibit high conductivities in both oxidising and reducing atmospheres are in high demand for solid oxide fuel cells (SOFCs) and solid oxide electrolytic cells (SOECs).", "In this paper, we investigated Cu-doped SrFe0.9Nb0.1O3−δ finding that the primitive perovskite oxide SrFe0.8Cu0.1Nb0.1O3−δ (SFCN) exhibits a conductivity of 63 Scm−1and 60 Scm−1 at 415 °C in air and 5%H2/Ar respectively.", "It is believed that the high conductivity in 5%H2/Ar is related to the exsolved Fe (or FeCu alloy) on exposure to a reducing atmosphere.", "To the best of our knowledge, the conductivity of SrFe0.8Cu0.1Nb0.1O3−δ in a reducing atmosphere is the highest of all reported oxides which also exhibit a high conductivity in air.", "Fuel cell performance using SrFe0.8Cu0.1Nb0.1O3−δ as the anode, (Y2O3)0.08(ZrO2)0.92 as the electrolyte and La0.8Sr0.2FeO3−δ as the cathode achieved a power density of 423 mWcm−2 at 700 °C indicating that SFCN is a promising anode for SOFCs.", "Solid oxide fuel cells (SOFCs) are electrochemical devices used to convert chemical energy into electricity with a very high efficiency1.", "Symmetrical fuel cells have the potential application to be used as reversible SOFCs, which can operate in both fuel cell and electrolyser modes.", "In a recent report, it was found that a much better stability can be achieved by SOFCs which operate in both SOFC and solid oxide electrolytic cell (SOEC) modes (reversible SOFC)2.", "For reversible SOFCs, the use of a symmetrical electrode such as (La0.75Sr0.25)Cr0.5Mn0.5O3−δ (LSCM) would be an ideal solution345.", "An essential requirement of the electrode material is that it must exhibit a high conductivity in both air and fuel conditions at the fuel cell operating temperature.", "Therefore, electrode materials exhibiting high conductivities in both oxidising and reducing atmospheres are in high demand for solid oxide fuel cells (SOFCs) and solid oxide electrolytic cells (SOECs), particularly for symmetrical SOFCs.", "There are plenty oxide materials which exhibit high conductivity in air.", "The real challenge is to identify a good stable oxide anode material exhibiting high conductivity in a reducing atmosphere56.", "Several redox stable mixed oxide-ion electronic conductors have been developed as ceramic anode materials for SOFCs, such as (La0.75Sr0.25)Cr0.5Mn0.5O3−δ (LSCM)7, Sr2MgMoO6−δ (SMMO)8, La4Sr8Ti11Mn0.5Ga0.5O37.5 (LSTMG)9, La0.8Sr0.2Sc0.2Mn0.8O3−δ (LSSM)10, La0.7Ca0.3CrO3−δ11, Sr2Fe1.5Mo0.5O6−δ1213; Pr0.8Sr1.2(Co,Fe)0.8Nb0.2O4+δ/CoFe alloy14, PrBaMn2O5+δ15, La0.33Sr0.67Ti0.33Mn0.67O3−δ (LSTM)16, Ce0.6MN0.3Fe0.1O2-La0.6Sr0.4Fe0.9Mn0.1O3 (CMF-LSFM)17.", "All of these oxides or composite anodes are redox stable or redox reversible.", "However, except for La-doped SrTiO3, the conductivity at the anode is typically below 30 S/cm.", "The anode conductivity needs to be further improved, particularly for tubular SOFCs with a long pathway for electrons.", "The conductivity of La-doped SrTiO3 in a reducing atmosphere is high if pre-reduced at a high temperature.", "However, the conductivity of doped SrTiO3 in air is generally less than 0.1 S/cm6918.", "In reported perovskite oxides, besides LSCM, The double perovskite Sr2Fe1.5Mo0.5O6−δ (SFMO), was demonstrated to be a good electrode for symmetrical SOFCs1213.", "However, the conductivity of SFMO under the SOFC anode environment is not very high thus further improvements are required13.", "On the other hand, a promising family of redox stable anodes for SOFCs is B-site doped SrFeO3−δ.", "It has been reported that SrFe1-xTixO3−δ where x = 0.3, 0.4 combined with Ce0.9Gd0.1O2−δ performs well as an anode for SOFCs19.", "It was found that SrFe0.9Ti0.1O3−δ is redox stable with a conductivity of 2.53 S/cm at 600 °C in a reducing atmosphere20.", "Anikina et al. investigated the conductivity of SrFe1−xNbxO3−δ, where x = 0.05, 0.1, 0.2, 0.3, 0.4 and it was found SrFe0.9Nb0.1O3−δ exhibits the highest conductivity in a reducing atmosphere.", "However, the conductivity is still below 1 S/cm at temperatures below 800 °C21.", "In this study, we re-investigated the conductivity of SrFe0.9Nb0.1O3−δ finding that its conductivity in a reducing atmosphere was ~30 S/cm which is much higher than the reported values.", "It was also found that partial replacement of Fe by Cu in SrFe0.9Nb0.1O3−δ can further increase the conductivity in a reducing atmosphere.", "The perovskite oxide SrFe0.8Cu0.1Nb0.1O3−δ (SFCN) exhibits a conductivity of 63 Scm−1 and 60 Scm−1 at 415 °C in air and 5%H2/Ar respectively.", "To the best of our knowledge, the conductivity of SrFe0.8Cu0.1Nb0.1O3−δ in a reducing atmosphere is the highest among reported oxide anodes for SOFCs which also exhibit a high conductivity in air.", "A SOFC using SrFe0.8Cu0.1Nb0.1O3−δ as the anode and La0.8Sr0.2FeO3−δ as the cathode has been fabricated with a good performance in hydrogen achieved at temperatures below 700 °C.", "Structure of New Oxides SrFe0.9−xCuxNb0.1O3−δ (x = 0–0.4) X-ray diffraction of SrFe0.9−xCuxNb0.1O3−δ (x = 0–0.4) showed that it exhibited a single phase cubic perovskite structure (SG: Pm-3m) for all compounds (Figure S1).", "The XRD pattern of the SrFe0.8Cu0.1Nb0.1O3−δ sample is shown in Fig. 1A.", "The increase in the copper content significantly reduced the sintering temperature of the material, with the formation of a single phase perovskite structure that was not observed for SrFe0.4Cu0.5Nb0.1O3−δ.", "Reitveld refinement of the structure using GSAS22 demonstrated a pseudo-linear increase in the lattice parameters with increased copper doping up to SrFe0.6Cu0.3Nb0.1O3−δ (Figure S3 and Table S2).", "The increase in lattice parameters with increasing copper content can be attributed to the larger ionic radius of copper compared to iron (Cu2+0.73 Å, Fe3+0.645 Å, Fe4+0.585 Å)23.", "Samples SrFe0.6Cu0.3Nb0.1O3−δ and SrFe0.5Cu0.4Nb0.1O3−δ exhibit similar lattice parameters whilst no impurity peaks can be observed on the XRD patterns, this is thought to be due to the proximity of the solid solution limit.", "Therefore the limit for achieving single phase in the SrFe0.9−xCuxNb0.1O3−δ series lies at x ≤ 0.5.", "The SEM picture of SrFe0.8Cu0.1Nb0.1O3−δ prepared by the solid state reaction method is shown in Fig. 2A.", "Thermogravimetric analysis of SrFe0.9−xCuxNb0.1O3−δ (x = 0–0.4) in air showed a minor total loss in weight for all compounds, between 0.2 wt% and 0.5 wt%, with no observable trend on increasing the dopant level, (Figure S3A).", "Accelerated weight loss was observed for all compounds on heating between 500 and 800 °C, with the weight loss noted to be reversible upon cooling.", "This acceleration in weight loss is likely to be the result of oxygen loss through high temperature reduction.", "Differential scanning calorimetry, Figure S3B, exhibits a reversible transition for all copper doped compounds, between 600 °C and 670 °C on heating and between 670 °C and 590 °C on cooling which could be related to high temperature phase transition24.", "Conductivity of New Oxides SrFe0.9−xCuxNb0.1O3−δ (x = 0–0.4) in Air The conductivity of the electrode materials is a key parameter to consider when evaluating their use in SOFCs.", "Whilst minimal copper doping, forming SrFe0.8Cu0.1Nb0.1O3−δ, elicits a significant increase in conductivity in air over SrFe0.9Nb0.1O3−δ, additional copper doping is observed to reduce the conductivity of the materials, although increasing dopant levels do not elicit a linear response in the reduction in conductivity (Fig. 3A).", "The introduction of Cu2+ dopant is expected to increase the average charge of iron in the sample with the proportion of Fe4+ ions, increasing the number of charge carriers and thus, in theory, increasing the conductivity25.", "Assuming that the copper dopant does not directly contribute to electronic conduction, the increase in the charge carrier concentration is only proportional to the iron content of the compound, which reduces with increasing Cu2+ dopant concentration.", "Thus at higher Cu2+ dopant concentrations the increase in charge carriers through the average charge of iron increasing is outweighed by the reduction in charge carriers through the reduction of the iron content leading to reduced conductivity.", "On the conductivity curves, a semiconductor-metal transition was observed for all compounds, with an increase in the transition temperature noted with increasing copper dopant levels (Fig. 3A).", "This transition has been observed previously for strontium ferrites, with Poulsen et al.26 suggesting that compound reduction at high temperature, resulting in a reduction in the charge carriers, was the cause of the transition.", "A pseudo-linear reduction in the oxygen content of strontium ferrite in air above 400 °C with increasing temperature, which would appear to confirm compound reduction at these temperatures, was observed previously27.", "The increase in the conductivity with increasing temperature was determined by Patrakeev et al. to be offset by the reduction in charge carrier concentration, causing an overall reduction in the electronic conductivity with increasing temperature, resulting in the pseudo-metallic behaviour28.", "Stability of New Oxides SrFe0.9−xCuxNb0.1O3−δ (x = 0–0.4) In order to investigate the stability of SrFe0.9−xCuxNb0.1O3−δ (x = 0–0.4) in a reducing atmosphere, STA analyses in 5%H2/Ar was carried out on the samples.", "The observed weight loss upon reduction of SrFe0.9−xCuxNb0.1O3−δ (x = 0–0.4) varies between 2.6% and 3.3%, with no observed trend with increasing dopant concentration (Figure S4A).", "Differential scanning calorimetry exhibits non-reversible transitions on heating for all compounds between 600 °C and 670 °C, associated with cationic reduction (Figure S4B)20.", "With the increase of copper dopant, the exothermic peaks happened at lower temperature indicating the reduction at lower temperature thus they are likely less stable, this has been confirmed by the XRD study (Fig. 1B).", "After reducing in 5%H2/Ar at 700 °C for 10 hours, it was found that the Cu-free sample SrFe0.9Nb0.1O3−δ was redox stable.", "For sample SrFe0.8Cu0.1Nb0.1O3−δ, the majority of the phase is perovskite whilst an extra peak at ~45 degree was observed which belongs to the strongest (110) peak of α-Fe (PDF: 6–696) after the reduction at 700 °C29.", "The formation of a Fe-rich FeCu alloy cannot be ruled out but the Cu content must be very low otherwise the peak should shift to a higher d-spacing.", "The exsolution of metal particles is further confirmed by SEM observation where a small particle of iron was exsolved on the surface after the reduction (Fig. 2B).", "The very weak peak at ~32.5° could be a peak for a solid solution based on Sr2Fe2O5+δ parent phase30.", "When x is increased to 0.2, the majority of sample SrFe0.7Cu0.2Nb0.1O3−δ is possibly Sr2Fe2O5+δ solid solution while an extra peak at ~43° was observed which could be the strongest peak of Cu (Fm-3m)31.", "Again, formation of a Cu-rich FeCu alloy is also possible with the presence of Fe at the B-site of the perovskite phase.", "At x = 0.3, 0.4, Sr2Fe2O5+δ based solid solution is the major phase with the Fe or Fe-rich alloy also present.", "The exsolution of metal seems strongly related to the composition, which will require further investigation.", "To exam whether the exsolution of metal is reversible, the reduced SrFe0.8Cu0.1Nb0.1O3−δ sample was re-oxidised in air at 1300 °C for 15 hours then further reducing in 5%H2/Ar at 700 °C for 10 hours and stop at the re-oxidation stage after 3 cycles.", "It was observed that the exsolved metal was ‘adsorbed’ back after re-oxidation ii air at high temperature (Fig. 2C) while it was exsolved out after further reduction in 5%H2/Ar at 700 °C for 10 hours (Fig. 2D).", "This indicate the process for exsolved metal is reversible as observed in other oxides3233.", "Conductivity of New Oxides SrFe0.9−xCuxNb0.1O3−δ (x = 0–0.4) in 5%H2/Ar To measure the conductivity in a reducing atmosphere, the SrFe0.9−xCuxNb0.1O3−δ pellets were coated with silver electrodes on both sides then reduced in 5%H2/Ar at 700 °C for 10 hours (Fig. 3B).", "The conductivity was measured in 5%H2/Ar on cooling.", "The highest conductivity for the samples measured was found to be for the SrFe0.8Cu0.1Nb0.1O3−δ sample with a conductivity of about 30–60 S/cm, in a reduced atmosphere.", "This is possibly due to the presence of exsolved Fe particles leading to increased electronic conductivity thus the total conductivity was also high.", "The lowest conductivity was observed for sample SrFe0.7Cu0.2Nb0.1O3−δ, due to the Sr2Fe2O5+δ based solid solution being the major phase.", "This indicates that the conductivity of Sr2Fe2O5+δ based solid solution is lower than the primitive perovskite oxide based on SrFeO3−δ.", "When x increased to 0.3 and 0.4, the intensity of the peak at ~45 ° which represents the exsolved Fe is obviously stronger than that for sample SrFe0.8Cu0.1Nb0.1O3−δ (Fig. 1B) even though the major phase was the Sr2Fe2O5+δ based solid solution.", "The conductivity of SrFe0.6Cu0.3Nb0.1O3−δ is comparable to that for the Cu-free sample SrFe0.9Nb0.1O3−δ whilst the conductivity of sample SrFe0.5Cu0.4Nb0.1O3−δ is slightly higher (Fig. 3B) due to higher concentration of exsolved Fe (or Fe-rich alloy).", "In the investigated oxides, in terms of both redox stability and conductivity, sample SrFe0.8Cu0.1Nb0.1O3−δ is the best.", "For comparison, the conductivity of sample SrFe0.8Cu0.1Nb0.1O3−δ in a reducing atmosphere is plotted together with the reported best oxide anodes for SOFCs (Fig. 3C).", "It is the highest among the reported materials with reasonably high conductivity in air and a conductivity two times greater than that of the Pr0.8Sr1.2(Co,Fe)0.8Nb0.2O4+δ/CoFe alloy14.", "The conductivities of all other reported oxide anode materials in a reducing atmosphere are lower than 30 S/cm.", "This is clearly shown when the conductivity is plotted at absolute value (Figure S5).", "High conductivity is very important for SOFCs due to some designs involving long pathways for electrons at the electrode.", "Both SFCN and Pr0.8Sr1.2(Co,Fe)0.8Nb0.2O4+δ/CoFe alloy have exsolved metal under reduction indicating that designing a material with exsolved metal under reduction will help to achieve a high conductivity in a reducing atmosphere.", "The exsolved metal may also improve the catalytic activity under the fuel cell operating conditions3435.", "Fuel Cell Performance when SrFe0.8Cu0.1Nb0.1O3−δ Was Used as the Anode Solid oxide fuel cells with a SrFe0.8Cu0.1Nb0.1O3−δ anode, YSZ electrolyte and La0.8Sr0.2FeO3−δ cathode were fabricated.", "The performance and the corresponding A.C. impedance spectra of hydrogen/air fuel cell at different temperatures are shown in Fig. 4A,B.", "Good fuel cell performance with a power density of 423 mW/cm2 was observed at 700 °C.", "The total polarisation resistance of the electrode at 700 °C was only 0.25 Ω cm2 indicating SrFe0.8Cu0.1Nb0.1O3−δ performs well as an anode for SOFCs.", "However, a small amount of Ru/CeO2 was introduced to improve the catalytic activity.", "For comparison, a SOFC with the same electrolyte and cathode was assembled with the Cu-free anode SrFe0.9Nb0.1O3−δ used instead of the Cu doped anode.", "As shown in Fig. 4C,D, the highest power density at 700 °C was 372 mW/cm2 which was slightly lower than that for a SOFC with SrFe0.8Cu0.1Nb0.1O3−δ anode.", "The total electrode polarisation was 0.30 Ω cm2 at 700 °C.", "The series resistance was 0.54 Ω cm2 which is also slightly higher than that of the cell where the SrFe0.8Cu0.1Nb0.1O3−δ anode was used (0.50 Ω cm2) (Fig. 4B,D).", "This indicates that the high conductivity of SrFe0.8Cu0.1Nb0.1O3−δ reduces both series and electrode polarisation resistances leading to high fuel cell performance.", "It should be noted that the exsolved Fe (or Fe rich FeCu alloy) at the SrFe0.8Cu0.1Nb0.1O3−δ anode may also improve the anode catalytic activity resulting in lower electrode polarisation resistance.", "The Arrhenius plot area-specific resistances (ASRs) for non-ohmic resistance of SrFe0.9Nb0.1O3−δ and SrFe0.8Cu0.1Nb0.1O3−δ anodes are shown in Figure S6.", "At 600 °C, the ASR for the two oxide anodes are similar but the ASR for SrFe0.8Cu0.1Nb0.1O3−δ is much lower at 650 and 700 °C indicating better catalytic activity.", "Copper, copper alloy and iron alloy has been widely studied as excellent anode catalysts in SOFCs636373839.", "In an early reported, it was found that FeCo alloy was exsolved from Pr0.4Sr0.6Co0.2Fe0.7Nb0.1O3−δ anode while excellent fuel cell performance has been achieved although the conductivity of this material was not presented40.", "Conclusions In this work, a conductive perovskite oxide SrFe0.8Cu0.1Nb0.1O3−δ has been identified which exhibits the highest conductivity in a reducing atmosphere for oxides which also exhibit a high conductivity in air.", "This high conductivity is probably related to the exsolution of Fe (or Fe-rich FeCu alloy) during the high temperature reducing process.", "After the reduction, besides the exsolved metal, the major phase is that of the perovskite.", "Good performance at intermediate temperatures in solid oxide fuel cells using the SrFe0.8Cu0.1Nb0.1O3−δ based anode indicates that it is a promising anode for SOFCs.", "This study indicates that the conductivity of the oxides with exsolved metal is significantly high.", "This provides a strategy to identify a good material with high conductivity in both air and reducing atmospheres, i.e., starting from an oxide material with high conductivity in air, followed by introducing transition elements such as Fe, Co, Ni, Cu in the lattice which may be exsolved from the lattice on reduction therefore resulting in high conductivity in a reducing atmosphere.", "Methods Synthesis of oxides SrFe0.9−xCuxNb0.1O3−δ (x = 0–0.4) were synthesised by a sol-gel process, similar to previously reported processes20.", "A stoichiometric amount of C4H4NNbO9·xH2O (99.9%, Sigma Aldrich) was dissolved in distilled water.", "H2O2 was added to the niobium solution until a colour change was elicited.", "Citric acid (99+%, Alfa Aesar), in a 2:1 molar ratio to the metal ions in the final product, was added and heated till a solution was formed.", "Stoichiometric amounts of Sr(NO3)2 (98%, Alfa Aesar), Fe(NO3)3·9H2O (98%, Alfa Aesar) and Cu(NO3)2·2.5 H2O (ACS grade, Alfa Aesar) were dissolved in distilled water.", "The solutions were mixed first then heated until gelation.", "The resultant gel formed was fired at 600 °C for 2 hours and further fired at 1200–1300 °C for 4–24 hours.", "The as-prepared powders were uniaxially pressed at 221 MPa in to pellets (ø ≈ 13 mm × 2 mm) and subsequently sintered in air at 1200 °C–1450 °C for 4–10 hours.", "The details are listed in Table S1.", "Analytical Procedures X-ray data was collected on a PANanalyticalX’Pert Pro in the Bragg-Brentano reflection geometry with a Ni-filtered Cu Kα source (1.5405 Å), fitted with a X’Celerator detector and an Empyrean CuLFF xrd tube.", "Absolute scans in the 2θ range of 5–100° with step sizes of 0.0167° were used during data collection.", "GSAS22 software was used to perform a least squares refinement of the lattice parameters of all the samples.", "Thermal analysis was conducted using a Stanton Redcroft STA 1500 Thermal Analyser on heating from room temperature to 800 °C and on cooling from 800 °C to room temperature in air, with a heating/cooling rate of 10 °C/min, and in 5% H2/Ar, again with a heating/cooling rate of 10 °C min−1, and with a flow rate of 5% H2/Ar of 50 mLmin−1.", "Scanning electron mircroscopy (SEM) measurements were carried out on a ZEISS SUPRA 55-VP Field Emission Scanning Electron Microscope.", "The densities of the pellets were determined from the measured mass and volume.", "Theoretical densities were calculated using experimental lattice parameters and the chemical formula SrFe0.9−xCuxNb0.1O3−δ (x = 0–0.4).", "The relative density of the pellets was 80–90% for all compounds.", "Conductivity Testing The pellets (ø ≈ 13 mm × 2 mm) were coated on opposing sides using silver paste for all samples.", "The conductivity of the samples was measured primarily in air between 300 °C to 700 °C.", "Secondary measurements over the same temperature range were conducted in 5% H2/Ar following an equilibration step of 10 hours at 700 °C in 5% H2/Ar.", "Measurements were conducted using a pseudo four-terminal DC method using a SolartronCell 1470E electrochemical interface controlled by CellTest software with an applied current of 1 - 0.1 A.", "Fuel Cell Fabrication and Testing The electrolyte support cell used in this study was prepared through a tape casting process, with the outer two layers having pore formers.", "A dense YSZ slurry was prepared by mixing YSZ powder with methyl ethyl ketone and ethanol, and along with binders (polyvinyl butyral and polyethylene Glycol).", "Porous YSZ was prepared by adding YSZ powder with methyl ethyl ketone and ethanol, binders (polyvinyl butyral and polyethylene Glycol) and graphite (UCP-2 grade, Alfa Aesar) sequentially.", "The resultant two slurries were tape-casted separately.", "The porous–dense–porous YSZ structure was prepared by laminating three green tapes, followed by sintering at 1500 °C for 4 h, after which the porosity was approximately 65%.", "The final thicknesses of the dense electrolyte and porous electrode were ~100 μm and 45 μm, respectively.", "The diameter of the porous YSZ region was 0.67 cm.", "To prepare composites of SFN-YSZ and SFCuN-YSZ electrolyte supported cell, the precursor solutions were firstly prepared by dissolving nitrate salts of Sr, Fe, Cu, and Nb in distilled water with the addition of quantitative amounts of citric acid.", "The SFCuN -YSZ anode was prepared by infiltrating the precursor aqueous solution into the anode side of the three-layered YSZ backbone.", "SFCuN was infiltrated into then porous YSZ backbone by a multi-step process followed by heating at 450 °C to decompose nitrates and citric acid.", "The infiltration process was repeated until 40 wt% loading of the oxide was achieved.", "Finally, SFCuN-YSZ anode wafers were calcined in air at 1000 °C.", "The LSF (La0.8Sr0.2FeO3−δ)-YSZ cathode was fabricated by infiltration using an aqueous solution of nitrate salts of La, Sr and Fe on a porous YSZ backbone opposite the anode layer.", "This was then calcined in air at 850 °C. 2 wt% Ru and 10 wt% ceria were also infiltrated into the anode and heated in air at 450 °C.", "For fuel cell performance tests, the cells were mounted on alumina tubes with ceramic adhesives (Ceramabond 552, Aremco).", "Ag paste and Ag wire were used for the electrical connections to both the anode and the cathode.", "The entire cell was placed inside a furnace and heated to the desired temperature.", "V–i polarization curves were measured using a Potentiostat in the temperature range of 700–600 °C.", "The fuel cell performance was measured by a Solartron 1470e Electrochemical Interface coupled with a Solartron 1455 controlled by electrochemical software Solartron CellTest.", "The a.c. impedance was measured in the frequency range between 1 MHz and 0.01 Hz at the amplitude of the a.c. signal 20 mV.", "Additional Information How to cite this article: Lan, R. et al.", "A perovskite oxide with high conductivities in both air and reducing atmosphere for use as electrode for solid oxide fuel cells.", "Sci.", "Rep. 6, 31839; doi: 10.1038/srep31839 (2016)." ]

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[ "Enhanced methane steam reforming activity and electrochemical performance of Ni0.9Fe0.1-supported solid oxide fuel cells with infiltrated Ni-TiO2 particles Enhanced methane steam reforming activity and electrochemical performance of Ni0.9Fe0.1-supported solid oxide fuel cells with infiltrated Ni-TiO2 particles LiKai1JiaLichao2WangXin2PuJian2ChiBoa2LiJian2 1School of Materials Science and Engineering, Xi’an Shiyou University, Xi’an 710065, China 2Center for Fuel Cell Innovation, State Key Laboratory for Materials Processing and Die & Mould Technology, School of Materials Science and Engineering, Huazhong University of Science and Technology, Wuhan 430074, China achibo@hust.edu.cn 35981 Ni0.9Fe0.1 alloy-supported solid oxide fuel cells with NiTiO3 (NTO) infiltrated into the cell support from 0 to 4 wt.% are prepared and investigated for CH4 steam reforming activity and electrochemical performance.", "The infiltrated NiTiO3 is reduced to TiO2-supported Ni particles in H2 at 650 °C.", "The reforming activity of the Ni0.9Fe0.1-support is increased by the presence of the TiO2-supported Ni particles; 3 wt.% is the optimal value of the added NTO, corresponding to the highest reforming activity, resistance to carbon deposition and electrochemical performance of the cell.", "Fueled wet CH4 at 100 mL min−1, the cell with 3 wt.% of NTO demonstrates a peak power density of 1.20 W cm−2 and a high limiting current density of 2.83 A cm−2 at 650 °C.", "It performs steadily for 96 h at 0.4 A cm−2 without the presence of deposited carbon in the Ni0.9Fe0.1-support and functional anode.", "Five polarization processes are identified by deconvoluting and data-fitting the electrochemical impedance spectra of the cells under the testing conditions; and the addition of TiO2-supported Ni particles into the Ni0.9Fe0.1-support reduces the polarization resistance of the processes ascribed to CH4 steam reforming and gas diffusion in the Ni0.9Fe0.1-support and functional anode.", "On-cell methane (CH4) reforming in Ni-based anodes is an attractive option for directly using CH4-based fuels for solid oxide fuel cells (SOFCs) with high fuel efficiency and simplified system design12.", "CH4 steam reforming is a catalytic process for commercial production of H2 or syngas at a H2:CO molar ratio of 3:1 according to the endothermic reaction of Excessive addition of H2O will further converts CO to CO2 by the slightly exothermic water gas shift (WGS) reaction345.", "If these reactions are taking place in the anode of an SOFC, H2 is consumed via electrochemical oxidation to generate electrical power67, forming by-product of H2O.", "Such in-situ formed H2O is simultaneously used for CH4 steam reforming, which reduces the amount of externally added H2O to improve the electrical efficiency of the SOFC system.", "However, for on-cell CH4 reforming in Ni-based anodes, coking is frequently observed in the anode when steam/carbon (H2O/CH4) ratio is low, since Ni catalyzes CH4 decomposition that produces deposited carbon in the form of filament or particle via either CH4 cracking or the Boudouard reactions as follow The soot-like carbon particles are distributed on the surface of Ni particles, occupying the active sites for electrochemical reaction and the pores for fuel gas transport8; and the carbon filaments formed by carbon diffusion into/precipitation out the Ni particles9 disintegrate the Ni-cermet anode by lifting out the Ni particles from the anode (dusting).", "It has been demonstrated that infiltration of oxides, such as rare-earth doped CeO2101112, BaO13 and CaO-MgO14, into the Ni-based anode is an effective way to enhance its coking resistance by suppressing carbon formation and promoting steam-carbon reactions.", "Although TiO2 has not been investigated in SOFCs, it was used as a support in catalysts for steam reforming of hydrocarbons (methanol15, ethanol16 and glycerol17), CO2 reforming of CH41518 and CO oxidation19; and high coking resistance was demonstrated in CH420 and ethanol16 reforming.", "Stimulated by these investigations, TiO2 was evaluated in direct-CH4 SOFCs for the enhancement of CH4 on-cell reforming in the present study.", "Compared with electrolyte- and electrode-supported SOFCs, metal-supported SOFCs have some advantages in the aspects of electrical/thermal conductivity and mechanical ductility; consequently, the temperature distribution in and tolerance to thermal cycle of the cell are improved2122.", "In our previous study, Ni-Fe alloy-supported SOFCs were investigated with the purpose of using wet (3 vol.% H2O) CH4 as the fuel, and high performance (0.6 V at 0.4 A cm−2 and 650 °C for 50 h7) was achieved.", "However, the Ni0.9Fe0.1-support used was not fully resistant to carbon deposition, and carbon lumps were formed in its large pores.", "In order to develop metal-supported direct-hydrocarbon SOFCs, Ni0.9Fe0.1-supported SOFCs were prepared with NiTiO3 infiltrated into the Ni0.9Fe0.1-support.", "It was expected that NiTiO3 would be reduced into TiO2-supported Ni particles in H2 to enhance CH4 reforming activity and resistance to carbon deposition of the Ni0.9Fe0.1-supported cells.", "Results Materials and cell characterization Figure 1a–c show the XRD patterns of the as-synthesized and reduced NTO and co-fired powder mixture of NiO, Fe2O3 and NTO.", "The as-synthesized NTO demonstrated a perovskite structure of NiTiO3 (JCPDF# 76-0334), and the reduced product was a mixture of TiO2 (JCPDF# 21-1276) and Ni (JCPDF# 04-0850).", "Figure 1d shows EDS mappings of Ni, Ti and O for the mixture.", "It indicates that the bright granules in surface are identified by EDS as metallic Ni, and the dark areas rich in Ti and O.", "Based on this result, it is expected that the infiltrated NTO particles on the surface of the scaffold of the cell support be reduced into TiO2-supported Ni (0) particles.", "It was confirmed in our previous study7 that the sintered NiO-Fe2O3 cell support is consisted of two phases of NiO and NiFe2O4, and its reduced form is Ni0.9Fe0.1 alloy.", "With NTO powder added, the co-fired NiO-Fe2O3-NTO mixture contained NiO, NiFe2O4 and NTO (Fig. 1a), which indicates that NTO was chemically compatible with NiO and NiFe2O4 at temperatures up to 1000 °C and would remain as an independent phase in the scaffold of the sintered NiO-NiFe2O4 cell support.", "Shown in Fig. 2 is the SEM microstructure of the fractured cross-section of the reduced cell with Ni0.9Fe0.1-support.", "As observed previously7, the sintered NiO-NiFe2O4 cell support was reduced into a porous scaffold (58%) with a bimodal pore distribution.", "The average size of the large pores was around 10 μm, which is beneficial for fuel gas transport in the support to the functional anode; and the small pores within the stem of the scaffold give a high specific surface area that is beneficial for CH4 reforming reaction.", "The Ni-GDC functional anode was approximately 1αm thick and intimately in contact with the fully dense GDC electrolyte (~10 μm) and the porous cell support (~1 mm).", "The thickness of the BSCF-LSM cathode was averagely 15 μm.", "Figure 3 respectively present the microstructure of the sintered and reduced cell supports with various amounts of infiltrated NTO from 1 to 4 wt.% of the weight of the half cell (NiO-Fe2O3 anode-support | NiO-GDC anode | GDC electrolyte).", "Reforming activity of infiltrated Ni0.9Fe0.1-supports CH4 reforming in the Ni0.9Fe0.1-support is a chemical process that in situ produces H2, which is electrochemically oxidized on the functional Ni-GDC anode to generate electrical power with byproduct of steam via the reaction of Thus the reforming activity of the Ni0.9Fe0.1-support is of critical importance for the performance of the cell with on-cell CH4 reforming.", "Figure 4 shows the CH4 conversion rate and reforming product distribution at 650 °C in the Ni0.9Fe0.1-supports loaded with different amounts of TiO2-supported Ni particles.", "The initial values of CH4 conversion rate were approximately 50%, 55%, 58%, 61% and 60% for the Ni0.9Fe0.1-supports loaded with 0%, 1%, 2%, 3% and 4 wt.% of NTO (designated as 0NTO, 1NTO, 2NTO, 3NTO and 4NTO), respectively.", "This indicates that the addition of TiO2-suported Ni particles in the Ni0.9Fe0.1-support promoted its reforming activity with a limit of 3 wt.% NTO, more than which the conversion rate decreased, possibly due to the over-cover of the reforming active sites on the surface of the Ni0.9Fe0.1 scaffold by TiO2 and increased surface area of the small Ni particles for carbon deposition.", "The CH4 conversion rate of 0NTO, 1NTO, 2NTO and 4NTO decreased obviously with time after approximately 12 h, only which of 3NTO remained relatively stable during the testing period of 24 h.", "The main reforming products were H2, CO and CO2 (Fig. 4b–d), and their concentrations varied accordingly with the testing time.", "Cell performance The cells with NTO-infiltrated Ni0.9Fe0.1-supports were evaluated at 650 °C with wet CH4 (3 vol.% H2O) as the fuel; Fig. 5 shows their initial I-V-P curves.", "The open circuit voltage (OCV) of all the cells was around 0.78 V, due to the partial electronic conduction of GDC electrolyte23.", "The maximum power densities increased from 0.99 to 1.20 W cm−2 as the NTO loading was increased from 0 to 3 wt.%.", "Further increasing NTO loading to 4 wt.%, it decreased to 1.17 W cm−2.", "Figure 6 shows the initial impedance spectra of the cells under a current density of 0.4 A cm−2 (Fig. 6a), from which the ohmic (RO) and polarization (RP) resistances were determined, and the corresponding distributions of relaxation time (DRT, Fig. 6b)2425.", "The value of RO of each cell was similar, around 0.063 Ω cm−2, and that of RP varied in an opposite direction to the cell voltage and power density.", "This tendency of cell performance change with the amount of loaded NTO in the Ni0.9Fe0.1-support is consistent with that of the activity for CH4 steam reforming shown above, which suggests that cell performance improvement is due to the increased reforming activity of the Ni0.9Fe0.1-support and the consequent increase in the amount of H2 available for the anode reaction.", "The DRT G(τ) was associated with the impedance Z(w) by the following expression: Where G(τ) is defined as the DRT of impedance Z, τ is relaxation time, Z′ (∞) is the limitation of the real part of Z as angular frequency w approaches infinity.", "Consequently, impedance could be represented as series connection of infinite number of parallel polarization resistor G(τ)dτ and a capacitor τ/G(τ)dτ.", "For a more detailed description of DRT method and application were referred26.", "After the initial evaluation, all the cells were further tested at 650 °C and a constant current density of 0.4 A cm−2 for up to 96 h; the results are shown in Fig. 7.", "The improvement on cell performance durability is in consistence with that on CH4 steam reforming activity.", "The cells with 0NTO, 1NTO, 2NTO and 4NTO Ni0.9Fe0.1-supports performed 67, 78, 90 and 96 h before the sudden drop of the cell voltage; and the cell with 3NTO Ni0.9Fe0.1-support outperformed the others, degrading linearly at a slow rate of 0.5 mV h−1 during the testing period.", "Post-test examination confirmed that the sudden voltage drop at the end of the test was caused by cell disintegration due to dusting of the Ni0.9Fe0.1-support.", "The linear voltage decrease, at nearly the same rate for all the cells, may represent the intrinsic cell degradation that needs further understanding for mechanism, whereas the non-linear voltage decrease is attributed to carbon deposition in the Ni0.9Fe0.1-support and functional anode.", "Since the deposited carbon remained in the cell, its amount can be quantified from the temperature-programmed oxidation (TPO) profile of the post-test cells, as shown in Fig. 8.", "The area of CO2 peak, an indication of the amount of CO2 formed from deposited carbon, were 7.89 × 10−8, 6.93 × 10−8, 2.61 × 10−8 and 3.15 × 10−8 for the cells with 1NTO, 2NTO, 3NTO and 4NTO Ni0.9Fe0.1-supports, respectively.", "These values support the explanation of the durability testing results and indicate that the cell with 3NTO anode-support is the most resistant to carbon deposition among the cells investigated.", "Discussion According to previous studies1927, the effectiveness of TiO2 on improving reforming activity can be attributed to its enhanced capability of H2O adsorption and consequently the coking resistance.", "It is the H2O adsorbed on the catalyst that increases the reforming activity19; and the prevalent presence of subsurface defects of TiO2 in reduced atmosphere, such as oxygen vacancies and Ti interstitials, enhances H2O adsorption due to surface relaxation and charge localization.", "On-cell methane reforming, constant adsorption of H2O in anode will shift the equilibrium reaction of Eqs (1) and (2) in a forward direction.", "Therefore, H2 and CO2 concentration increases whereas CO concentration decrease with increase in the amount of H2O.", "The increase in H2 concentration and the decrease in CO concentration subsequently prevent possible carbon formation by shifting Boudard reaction (Eq. 3) and decomposition of CH4 (Eq. 4) in a backward direction.", "In addition, the excess H2 reacts with oxygen ion from electrolyte to product electrical power and steam, which enhances the water-gas shift reaction and retards CH4 decomposition.", "In additional to the contribution of H2O adsorption on TiO2, the TiO2-supported Ni particles on the surface of Ni0.9Fe0.1 scaffold are also considered to increase the reforming activity, due to its known tendency to form a strong metal-support interaction (SMSI) between TiO2 support and Ni metal and widely used catalyst of CH4 and ethanol steam reforming1628.", "Based on the DRT shown in Fig. 6b and the results reported in a previous investigation25, five polarization processes were identified for individual cells, which are two high-frequency processes ascribed to the gas diffusion and charge transfer/ionic transport within the functional anode (P2A and P3A), one high-frequency process associated with oxygen surface exchange and bulk diffusion within the BSCF-LSM cathode (P2C), one low-frequency process related to mass transport in the Ni0.9Fe0.1-support (P1A) and one low-frequency process attributed to CH4 reforming in the Ni0.9Fe0.1-support (PRef).", "The contribution of each process to the total polarization resistance was obtained by data fitting the impedance spectra (Fig. 6a) using the complex nonlinear least-squares method and an equivalent circuit (inset in Fig. 6a) consisting of an ohmic resistor RO, two RQ elements for P2A and P3A, a Gerischer element (G) for P2C, a generalized finite length Warburg element (W) for P1A and another RQ element for PR.", "The change of the polarization resistance for each process, R1A, R2A, R3A, R2C and RRef, with the amount of loaded NTO is demonstrated in Fig. 6c.", "R3A and R2C remained almost unaffected by NTO infiltration, since the cathode was identical for all the cells, and the electrochemical reaction in the functional Ni-GDC anodes was the same reaction of H2 oxidation25 regardless of the amount of NTO loaded in the Ni0.9Fe0.1-support.", "The resistance of diffusion of reformate in the Ni0.9Fe0.1-support and Ni-GDC functional anode, R1A and R2A, decreased with increasing NTO amount till 3 wt.% and then increased at 4 wt.%, which reflects the amount change of H2 in the reformate.", "It is expected that higher concentration of H2 in the reformate lead to lower diffusion resistance in porous cell support and functional anode due to the high diffusivity of H2.", "RRef is assigned to CH4 steam reforming process; its change with the amount of loaded NTO in the Ni0.9Fe0.1-support is consistent with that of the reforming activity.", "According to the data-fitting results and discussions, it may be concluded that the cell performance improvement with NTO infiltration in the Ni0.9Fe0.1-support is attributed to the improved CH4 reforming activity and the decreased potential of carbon deposition; consequently the polarization resistances related to CH4 reforming and reformate transport processes are decreased.", "NTO infiltration into Ni0.9Fe0.1-supports was investigated with the purpose of enhancing CH4 steam reforming activity, carbon deposition resistance and cell performance.", "Based on the obtained results and discussion, the following conclusions are drawn.", "The activity of the Ni0.9Fe0.1-support for CH4 steam reforming is enhanced by infiltrated NTO, which is reduced into TiO2-supported Ni (0) particles in H2.", "The TiO2 improves the resistance to carbon deposition by adsorbing H2O, while the supported small Ni particles promote CH4 decomposition. 3 wt.% of the weight of the half cell (anode-support | functional anode | electrolyte) is the optimal value for the amount of NTO infiltrated into the Ni0.9Fe0.1-support.", "Increased CH4 reforming activity lead to the improvement of cell performance, durability and resistance to carbon deposition.", "The overall cell polarization resistance is contributed by five polarization processes associated with CH4 reforming (Pref), mass transport in anode-support (P1A), gas diffusion in functional anode (P2A), charge transfer within functional anode (P3A), and oxygen surface exchange and bulk diffusion within cathode (P2C).", "The addition of NTO into the Ni0.9Fe0.1-support reduces the polarization resistance of Pref, P1A and P2A.", "Methods Cell fabrication Ni0.9Fe0.1-supported cells were fabricated by tape casting-screen printing-sintering process.", "NiO (Haite Advanced Materials) and Fe2O3 (Sinopharm) powders were mixed at a Ni:Fe molar ratio of 9:1 and ball-milled for 24 h in xylene/ethanol solvent with fish oil (Richard E.", "Mistler, Inc.) as the dispersant, corn starch as the pore former, poly vinyl butyral (Solutia Inc.) as the binder and butyl benzyl phthalate and poly alkylene glycol (Solutia Inc.) as the plasticizer.", "The prepared slurry was cast into a tape with a dry thickness of ~1.2 mm, which was then die-cut into discs (25 mm in diameter) as the cell support, on which NiO (Inco)-GDC (10 mol.% Gd-doped CeO2, NIMTE, CAS) functional anode and GDC electrolyte were screen printed in sequence, followed by sintering at 1450 °C in air for 5 h.", "La0.8Sr0.2MnO3-coated Ba0.5Sr0.5Co0.8Fe0.2O3 (LSM-BSCF) cathode29 was then screen-printed on the sintered GDC electrolyte and sintered in air at 1050 °C for 2 h.", "To introduce TiO2-supported Ni particles onto the stem of NiO-Fe2O3 scaffold (~40% porosity30), an aqueous solution containing Ti and Ni ions at the stoichiometric concentration of NiTiO3 (NTO) was prepared as follow.", "Tetrabutyl titanate (C16H36O4Ti, Sinopharm) was dissolved in a dilute nitric acid aqueous solution under stirring, and then stoichiometric amount of Ni nitrate (Ni(NO3)2·6H2O, Sinopharm) was added prior to the addition of citric acid (CA) and ethylenediamine tetraacetic acid (EDTA) as the chelants.", "The molar ratio of metal ions:CA:EDTA in the solution was 1:1:1.5.", "Ammonia solution was used to adjust the pH value of the solution to approximately 7.", "Such prepared solution was infiltrated into the pores of the sintered NiO-Fe2O3 scaffold and calcined in air at 1000 °C for 2 h to form crystallized NTO nano particles.", "This infiltration process was repeated to achieve the desired amounts of loaded NTO in the scaffold.", "The crystal structure of NTO and its chemical reactivity with NiO and Fe2O3 were determined by X-ray diffraction (XRD, X’Pert) using a NiO-Fe2O3-NTO powder mixture co-fired in air at 1000 °C for 2 h.", "The NTO powder was obtained by calcining the dried solution in air at 1000 °C for 2 h, and its reduced form (650 °C in H2 for 2 h) was characterized by XRD for phase identification and examined by using a scanning electron microscope (SEM, FEI sirion 200).", "Steam reforming activity evaluation To evaluate the catalytic activity of the infiltrated Ni0.9Fe0.1-support for CH4 steam reforming, the NiO-Fe2O3 support sintered at 1450 °C in air for 5 h was sealed in a ceramic housing using a CeramabondTM sealant (Aremco Product, Inc.) and reduced at 650 °C in H2 for 2 h.", "Then a mixture of 10% CH4, 10% H2O and 80% He was fed into the porous support at a constant rate of 100 ml min−1.", "The steam content in the mixture was controlled by flowing dry CH4 and He gases through a saturator containing distilled water at 50 °C according to the following equation31.", "Compositional analysis of the effluent gas from the reactor was conducted with an on-line Pfeiffer Vacuum Mass Spectrometer.", "The steam reforming was performed at temperatures between 500 and 700 °C, and the CH4 conversion rate (X (%)) was estimated using the following equation.", "Cell testing and characterization The cell performance was evaluated at 650 °C with wet (3 mol.% H2O) CH4 as the fuel and ambient air as the oxidant at a flow rate of 100 ml min−1.", "Using a power supply of Solartron 1480A in 4-probe mode, the current density (i)–voltage (V)-power density (P) polarization curves were obtained at a scanning rate of 5 mVs−1 from 0 to 1 V, and electrochemical impedance spectra (EIS) were acquired within a frequency range from 100 KHz to 0.01 Hz and an AC signal amplitude of 10 mV.", "The microstructure of the cell was examined by using a SEM.", "The resistance to carbon deposition of (the amount of deposited carbon in) the Ni0.9Fe0.1-supported cell was characterized by temperature-programmed-oxidation (TPO) method at a flow rate of 20 ml min−1 of pure oxygen.", "Additional Information How to cite this article: Li, K. et al.", "Enhanced methane steam reforming activity and electrochemical performance of Ni0.9Fe0.1-supported solid oxide fuel cells with infiltrated Ni-TiO2 particles.", "Sci.", "Rep. 6, 35981; doi: 10.1038/srep35981 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[ "A niobium and tantalum co-doped perovskite cathode for solid oxide fuel cells operating below 500 °C A niobium and tantalum co-doped perovskite cathode for solid oxide fuel cells operating below 500 °C LiMengran1ZhaoMingwen2LiFeng2ZhouWeia3 http://orcid.org/0000-0003-0322-095XPetersonVanessa K.4XuXiaoyong1ShaoZongping3GentleIan5ZhuZhonghuab1 1School of Chemical Engineering, The University of Queensland, St Lucia, Queensland 4072, Australia 2School of Physics and State Key Laboratory of Crystal Materials, Shandong University, Jinan 250100, Shandong, China 3Jiangsu National Synergetic Innovation Center for Advanced Materials (SICAM), State Key Laboratory of Materials-Oriented Chemical Engineering, College of Chemical Engineering, Nanjing Tech University, No. 5 Xin Mofan Road, Nanjing 210009, Jiangsu, China 4Australian Centre for Neutron Scattering, Australian Nuclear Science and Technology Organisation, Lucas Heights, New South Wales 2234, Australia 5School of Chemistry and Molecular Biosciences, The University of Queensland, St Lucia, Queensland 4072, Australia azhouwei1982@njtech.edu.cnbz.zhu@uq.edu.au 13990 The slow activity of cathode materials is one of the most significant barriers to realizing the operation of solid oxide fuel cells below 500 °C.", "Here we report a niobium and tantalum co-substituted perovskite SrCo0.8Nb0.1Ta0.1O3−δ as a cathode, which exhibits high electroactivity.", "This cathode has an area-specific polarization resistance as low as ∼0.16 and ∼0.68 Ω cm2 in a symmetrical cell and peak power densities of 1.2 and 0.7 W cm−2 in a Gd0.1Ce0.9O1.95-based anode-supported fuel cell at 500 and 450 °C, respectively.", "The high performance is attributed to an optimal balance of oxygen vacancies, ionic mobility and surface electron transfer as promoted by the synergistic effects of the niobium and tantalum.", "This work also points to an effective strategy in the design of cathodes for low-temperature solid oxide fuel cells.", "Sluggish activity of cathode materials impedes operation of solid oxide fuel cells at low temperatures.", "Here, the authors report a niobium and tantalum co-doped perovskite cathode exhibiting high electroactivity below 500 °C, and argue that the dopants improve the cathode performance synergistically.", "A low-temperature solid oxide fuel cell (LT-SOFC) is a durable energy device that can be deployed to convert the chemical energy stored in various types of fuels into electricity with high efficiency, ease of sealing, and reduced system and operational costs123.", "However, the low operating temperature (450-600 °C) typically leads to sluggish kinetics of the oxygen reduction reaction (ORR) at the cathode, with this being a major limitation to LT-SOFC performance456789.", "Intensive research has been carried out in an effort to explore cathode compositions suitable for operation at low temperature467101112131415.", "Oxides offering high mixed ionic and electronic conductivities (MIECs) are considered to be some of the most promising candidates for the next generation of SOFC cathodes due to their extended active sites for ORR when compared with purely electronic conducting materials1617.", "Some of these MIEC cathodes have been reported exhibiting relatively low cathode polarization resistance below 600 °C (ref. 11).", "For example, the in-situ co-assembly of La0.8Sr0.2MnO3 (with a very low O2 dissociation energy barrier) and Bi1.6Er0.4O3 (with fast oxygen incorporation kinetics) leads to a high performance nanocomposite cathode showing a low polarization resistance of ∼0.078 Ω cm2 and ∼0.6 Ω cm2 at 600 and 500 °C, respectively11.", "Choi et al.12 developed a novel MIEC cathode PrBa0.5Sr0.5Co1.5Fe0.5O5+δ that exhibits a polarization resistance as low as ∼0.33 Ω cm2 at 500 °C, and the NdBa0.75Ca0.25Co2O5+δ material also shows an outstanding ORR activity at reduced temperature7.", "Another MIEC cathode composition, Ba0.9Co0.7Fe0.2Mo0.1O3−δ, was also reported to show an enhanced cathode performance with a polarization resistance of ∼0.28 Ω cm2 at 500 °C (ref. 18).", "Currently, some of the most popular MIEC cathode materials are the stabilized SrCoO3−δ (SC) perovskite oxides, such as Sm0.5Sr0.5CoO3−δ (ref. 19), (La,Sr)(Co,Fe)O3−δ (refs 20, 21) and Ba0.5Sr0.5Co0.8Fe0.2O3−δ422, which are claimed to exhibit high ORR activity in the intermediate temperature range 600–750 °C because of their relatively high mixed conductivities2324.", "The perovskite structure of SC, which is favoured for ORR, is usually stabilized by partial B-site substitution with high oxidation-state cations25, such as Nb2627, Mo28, Sb2930 and P3132, and these cations lead to low area-specific resistances (ASRs) at reduced temperature272829313334.", "Besides the single doped SCs, Zhou et al.10 developed a highly active perovskite cathode material, featuring a partial replacement of Co ions with both Sc3+ and Nb5+, and these dopants induce a remarkably high ORR activity at 550 °C.", "To the best of our knowledge, few studies report the possible synergistic effects of co-doping highly charged dopants on catalysing the ORR in LT-SOFC cathodes.", "Herein, we report the study of the synergistic effects of two highly charged B-site dopants on the performance of the perovskite LT-SOFC cathode SrCo0.8Nb0.1Ta0.1O3−δ (SCNT), with this cathode exhibiting outstanding and stable electrochemical performance below 500 °C.", "A low ASR of ∼0.16 and ∼0.68 Ω cm2 is achieved at 500 and 450 °C, respectively, by the SCNT cathode in a symmetrical cell configuration under open circuit conditions.", "A LT-SOFC with a pure SCNT cathode exhibits good performance of ∼1.2 and ∼0.7 W cm−2 at 500 and 450 °C, respectively.", "Our results show that the co-substitution of Nb5+ and Ta5+ can lead to an optimized balance of oxygen vacancies, ionic mobility and surface electron-transfer, which potentially benefit the ORR in the SCNT cathode.", "Results Structure and cation arrangement of SCNT Joint Rietveld analysis of neutron and X-ray powder diffraction data (Fig. 1a,b) revealed that the SCNT at room temperature exhibits a cubic perovskite structure with space-group symmetry and a lattice constant of 3.9066(1) Å (Table 1).", "High-resolution transmission electron microscopy combined with selected area electron diffraction (SAED) (Fig. 1c) confirms this structure.", "Moreover, the binding energies of Nb 3d 5/2 (206.76 eV) and Ta 4f 7/2 (25.58 eV) in SCNT, obtained from X-ray photoelectron spectroscopy, indicate that the dopants are both in 5+ valence3536 (Supplementary Fig. 1).", "The cubic structure of SC is maintained by the co-doping of Nb5+ and Ta5+ at the Co-site likely because of their high oxidation states25.", "Rietveld refinement results show Nb and Ta cation doping levels of 9.7(5) and 6.9(5) mol%, respectively, and an oxygen deficiency level of 5.6(5) mol% in SCNT.", "Both the cubic perovskite structure and oxygen deficiency are beneficial for oxygen-ion conduction, which is critical for a cathode, particularly for LT-SOFC application.", "The former makes oxygen vacancies migrate freely among lattice-equivalent oxygen sites37, while the latter facilitates ionic conduction1638.", "ORR activity in symmetrical and single cells We determined the ORR activity of SCNT in a symmetrical cell configuration between 450 and 700 °C using electrochemical impedance spectroscopy (EIS).", "The cathode ASR, calculated from the intercept difference of EIS impedance with the real axis (that is, Re_Z in Fig. 2c), is the key variable characterizing the cathode performance, with low ASR indicating high activity.", "The intercept of the impedance at high frequencies indicates an ohmic resistance arising from the electrolyte, electrode and connection wires39, with only approximately 1–2% of the total ohmic resistance contributed from the SCNT cathode on both sides of the electrolyte Gd0.1Ce0.9O1.95 (GDC)-based symmetrical cell (Supplementary Fig. 2a).", "The compatibility of SCNT with Sm0.2Ce0.8O1.9 (SDC) and GDC electrolytes was examined by comparing the X-ray diffraction patterns of a 50:50 wt.% powder mixture of the SCNT and electrolyte after heating to the cathode fabrication temperature of 1,000 °C for 2 h (Supplementary Fig. 3).", "The results reveal no obvious changes to the SCNT after heating with electrolyte, indicating a good chemical compatibility between the two.", "Since the silver current collector does not significantly affect cathode performance40 and the cathode thickness (∼10 μm) proves to be sufficient (Supplementary Fig. 2b), our measured ASRs reflect the ORR activity of the SCNT cathode.", "Figure 2a shows that the SCNT cathode exhibits notably high ORR activity at low temperature, with an ASR as low as 0.061–0.086, 0.16–0.23 and 0.68–0.80 Ω cm2 at 550, 500 and 450 °C, respectively.", "The SCNT cathode outperforms the other reported cathode compositions at below 500 °C.", "(Supplementary Table 1)710111218404142 For example, the electroactivity of SCNT cathode is nearly twice that of the highly active SrSc0.175Nb0.025Co0.8O3−δ at 500 °C (ref. 10), and is also higher than that of Ba0.9Co0.7Fe0.2Mo0.1O3−δ at 450 °C (ref. 18).", "When examined against other cathodes, the SCNT cathode performance is also found to be higher than that of the isostructural SrCo0.9Nb0.1O3−δ (SCN10), SrCo0.9Ta0.1O3−δ (SCT10), SrCo0.8Nb0.2O3−δ (SCN20) and SrCo0.8Ta0.2O3−δ (SCT20) perovskite cathode materials (Supplementary Fig. 4), having ASRs of 0.476±0.009, 0.353±0.001, 0.63±0.08 (ref. 43) and 0.25±0.02 Ω cm2 (ref. 43), respectively, at 500 °C.", "In addition, a lower activation energy (103.1±0.8 kJ mol−1) of SCNT is observed relative to that of SCN10 (105.3±1.6 kJ mol−1), SCT10 (105.3±0.5 kJ mol−1), SCN20 (108.5±0.3 kJ mol−1) and SCT20 (105.8±1.5 kJ mol−1), implying its suitability for catalysing oxygen reduction at low temperature.", "The performance of the SCNT cathode in a LT-SOFC was evaluated using Ni-SDC|SDC (∼20 μm) |SCNT (∼10 μm; Supplementary Fig. 5a) and Ni-GDC|GDC (∼14 μm)| SCNT (∼10 μm) fuel cells (Fig. 2b).", "The micrographs of the two single-cell cross sections are shown in Supplementary Fig. 6.", "At 550, 500 and 450 °C, power densities of 1.13, 0.77 and 0.37 W cm−2 are achieved, respectively, in the former single cell (using SDC as the electrolyte) with ohmic resistances of ∼0.072, 0.113 and 0.193 Ω cm2, which mainly arise from the electrolyte.", "The electrode polarization resistance (the sum of cathode and anode ASRs) are ∼0.059, 0.132 and 0.271 Ω cm2 at the respective temperature.", "Given that SCNT has reasonable chemical compatibility with GDC (Supplementary Fig. 3b) and a similar ORR activity with both GDC and SDC electrolyte (Supplementary Fig. 2c), GDC was also used in single cells due to its ease of coating.", "The cell can generate a peak power density as high as 1.75, 1.22 and 0.7 W cm−2 at 550, 500 and 450 °C, respectively, this being significantly higher than that of Ba0.5Sr0.5Co0.8Fe0.2O3−δ of ∼0.97, 0.52 and 0.316 W cm−2, respectively (Supplementary Fig. 5b).", "With a thinner GDC electrolyte, the fuel cell ohmic resistance is reduced to 0.033, 0.049 and 0.083 Ω cm2 at these temperatures, less than half of that for the SDC (∼20 μm)-based fuel cell.", "However, the electrode resistance of the GDC cell is only slightly lower than that of the SDC-based cell, being 0.056, 0.116 and 0.242 Ω cm2 at these respective temperatures.", "Taking into consideration the ease and low-cost of the ceramic fabrication processes involved in the necessary scale-up5, GDC electrolyte fuel cells can be fabricated to a thickness of approximately 10–14 μm, though further reduction in GDC thickness is expected to boost the single cell performance by lowering its ohmic resistance69.", "Overall, the performance of the SCNT-based fuel cell surpasses the target of 500 mW cm−2 for SOFCs44, suggesting the possibility of practical operation even below 450 °C.", "Synergistic effects of Nb and Ta on the ORR Notably, SCNT shows a higher ORR activity when compared with the iso-structural SCN20 and SCT20 materials with similar lattice constants of 3.9066(1) Å for SCNT (Table 1), 3.8978(2) Å for SCT20 and 3.8971(1) Å for SCN20, obtained from the analysis of the neutron powder diffraction (NPD) data in our previous work43.", "The oxygen vacancy content of the SCN20, SCT20 and SCNT materials was also determined from NPD data to be 0.102±0.02, 0.159±0.15 and 0.168±0.15, respectively, revealing a similar oxygen vacancy level in SCNT and SCT20, which are both significantly higher than in SCN20.", "Thermal gravimetric analysis also shows higher oxygen vacancy contents in SCNT and SCT20 than in SCN20 at elevated temperature.", "(Supplementary Fig. 7) Given the fixed valence of dopants, the valence of reducible Co is likely the main reason for the oxygen vacancy concentration differences, and the average valence of cobalt in samples was calculated from the elemental composition determined from the structural refinement.", "The average valence of Co is 3.44, 3.33 and 3.41 for SCN20, SCT20 and SCNT, respectively.", "The lower Co valence in Ta-doped samples can be ascribed to the lower electronegativity of Ta than Nb43.", "In addition, our first-principles calculation results also show that oxygen formation energies are 1.539, 1.456 and 1.512 eV for the Nb-, Ta- and co-doped models, respectively, which further supports the observed relatively high oxygen deficiency in SCNT as induced by Ta.", "However, it seems insufficient to explain the better performance of SCNT than SCT20 merely by their oxygen vacancy contents.", "Given the similar particle size (Supplementary Fig. 8) but slightly lower electrical conductivity (Supplementary Fig. 9) of SCNT compared to SCN20 and SCT20, the superior cathode electroactivity of SCNT is likely attributable to other ORR-related properties such as bulk oxygen ionic conductivity and oxygen surface-exchange kinetics.", "Hence we estimated the ionic conductivity of the SCN20, SCT20 and SCNT materials by studying the oxygen permeability of dense membranes with similar dimensions from 600 to 475 °C.", "The higher ionic conductivity (Fig. 3a) of SCNT over SCN20 can be explained by the more oxygen vacancies in SCNT relative to SCN20.", "Ionic conductivity is also known to be significantly affected by other factors such as lattice geometry, critical radius45, and lattice free-volume available for oxygen ions to pass through46.", "Because SCNT and SCT20 have similar lattice dimensions, the faster ionic conduction in SCNT may stem from the synergistic effects of Nb and Ta, which potentially decrease the energy barrier for oxygen migration between neighbouring octahedral CoO6 vacancies, as reported for the Sc3+ and Nb5+-doped perovskite oxide by Zhou et al.10 In order to confirm this hypothesis, we investigated the pathways for oxygen vacancy migration through first-principles calculations.", "We found that our three models have very similar minimum energy pathway, as shown in Fig. 3b, but with different energy barriers.", "The highest energy barrier along the pathway is 0.433, 0.638 and 0.572 eV for Nb-, Ta- and the co-doped models, respectively, (Supplementary Table 2), indicating an easier vacancy mobility within the co-doped model as compared to Ta-doped model.", "Although SCNT and SCT20 have similar oxygen vacancy levels, the higher ionic conductivity of SCNT than SCT20 is likely a result of the incorporation of Nb that enhances ionic mobility in the lattice.", "Additionally, slightly lower electrical conductivity (σtotal) that includes both electronic and ionic conductivity (σion) is observed for SCNT than for SCN20 and SCT20 (Supplementary Fig. 9).", "The lower electrical conductivity of SCNT is caused by increased oxygen vacancies that can diminish the charge carriers for hopping process.", "The ionic transference number (tion=σion × σtotal−1) of SCNT, SCN20 and SCT20 was calculated and shown in Supplementary Fig. 10.", "As the electronic conductivity dominates, the ionic transference number is very small in the studied temperature range.", "Nevertheless, SCNT has a larger ionic transference number than SCN20 and SCT20; e.g.", "SCNT has a transference number of ∼1.33 × 10−5 at 500 °C, which is ∼2.7 and ∼2.1 times that of SCN20 and SCT20, respectively.", "By extending the oxygen reduction active region and enhancing the ORR kinetics4748, the higher oxygen vacancy content and improved mobility of SCNT imparted by the co-doping are likely to be more important than the electronic conductivity to the outstanding ORR performance of SCNT.", "The oxygen surface exchange kinetics were investigated by comparing the O2-intake time of each sample in response to an atmosphere change from N2 to air at 500 °C.", "The SCNT mass equilibrates faster (∼188 s) than SCN20 (∼245 s) and SCT20 (∼217 s), suggesting a faster oxygen surface exchange of SCNT at lower temperature (Supplementary Fig. 11).", "Therefore, the Nb and Ta together could also synergistically enhance the surface-exchange processes by creating more oxygen vacancies and improving ionic mobility.", "We also fitted the impedance spectra of SCNT, SCN20 and SCT20 cathodes to an equivalent circuit model consisting of two dominant reaction processes, with an example fitting presented in Fig. 2c.", "As shown in Supplementary Fig. 12 and from our previous work43, the cathode reciprocal resistances at high and low frequencies show different oxygen partial pressure dependencies m (as shown in equation (5)): m is ∼0.25 at high frequencies (HF) and ∼0.5 at low frequencies (LF) According to the relationship between pO2 dependencies and rate-determining-steps as discussed by other researchers495051, the polarization resistance at HF is likely related to charge transfer and that at LF to non-charge-transfer steps.", "Where O2,adsis an adsorbed oxygen molecule on the cathode surface, is an electron, is an oxygen vacancy and is an oxygen.", "Table 2 summarizes the polarization resistance of these two processes.", "SCNT exhibits significantly lower ASRs for the charge-transfer process than either SCN20 or SCT20, and nearly half of the resistance of SCN20 and similar resistance to SCT20 for the non-charge transfer process.", "The fast kinetics of charge transfer can be partly attributed to the high oxygen vacancy content of SCNT induced by Ta, since oxygen vacancies are shown to play an important role in the charge-transfer process (equation (1)).", "On the other hand, since Nb5+ and Ta5+ are inert to oxygen surface redox-processes due to their fixed valence, Co plays a vital role in catalysing the oxygen reduction.", "Therefore, we calculated the atomic orbital-resolved electron density of states projected onto the Co atom in Nb, Ta and Nb/Ta co-doped strontium cobalt oxides using first-principles calculations.", "As shown in the schematic models (Fig. 4c,f for Nb or Ta single-doped models and Fig. 4i for co-doped model), there are two categories of cobalt atoms: one is the nearest neighbour (NN) Co to the dopant, including Co1 and Co2 in the single-doped model, and Co1, Co2 and Co3 for co-doped model; the other is the next-nearest neighbour (NNN) Co to the dopants, including Co3 in the single-doped model and Co4 in the co-doped model.", "By comparing the electronic states of these Co atoms, we found that the NN-Co atoms have very similar density of states (DOS) near the Fermi level for these three models.", "For the NNN-Co atoms, the Ta-doped model (Fig. 4e) exhibits only 60% of DOS of the Nb-doped model (Fig. 4b) near the Fermi level, indicating that Nb is more favourable to increasing the DOS of the NNN-Co near the Fermi level.", "Due to the beneficial effect of Nb, the DOS of the NNN-Co near the Fermi level of the co-doped model (Fig. 4h) is ∼98% that of Nb-doped model.", "The enhanced DOS at the Fermi level can increase the efficiency of electron-transfer to the adsorbed oxygen species O2,ads (ref. 52), and it is therefore likely that the higher DOS of NNN-Co atoms near the Fermi level, as induced by Nb, is the reason for the faster kinetics of charge-transfer in SCNT than in SCT20, despite their similar oxygen vacancy concentration.", "Our experimental and calculation results reveal that the superior electroactivity of SCNT is a result of a balance of the oxygen vacancy content, oxygen-ion mobility and electron-transfer to O2,ads, which are imparted by co-doping Nb and Ta.", "Stability tests The durability of the cathode was investigated in both symmetrical and single cell configurations, as shown in Fig. 5.", "The ASR of SCNT in a symmetrical cell configuration was tested under the open circuit condition for ∼200 h.", "The ORR activity was relatively stable at ∼0.033 Ω cm2 with an ASR increase of ∼0.06% per hour during the testing period.", "The slight increase of the ASR during the stability test is likely to arise from the densification and reduced porosity of the silver current collector during this testing timeframe, which degrades the overall cathode performance535455.", "Another short-term stability evaluation of the SCNT cathode in a single-cell configuration with ∼20 μm-thick SDC electrolyte also showed that the SCNT is stable under 0.7 V polarization for at least 150 h at 450 °C in air.", "The low current density noted in the stability testing arises from the electrolyte thickness, which leads to high ohmic resistance.", "This stable ORR activity of SCNT is expected given its stable perovskite lattice (Supplementary Fig. 13).", "Discussion In summary, the perovskite composition SrCo0.8Nb0.1Ta0.1O3−δ (SCNT) was synthesized and exhibits the highest reported activity for the reduction of oxygen in an LT-SOFC, to the best of our knowledge, with an ASR of only ∼0.16 and ∼0.68 Ω cm2 at 500 and 450 °C, respectively, in a symmetrical cell configuration.", "High power density is therefore achieved using a pure SCNT cathode as a result of its outstanding ORR activity.", "A performance comparison amongst the iso-structural SCNT, SrCo0.8Nb0.2O3−δ (SCN20) and SrCo0.8Ta0.2O3−δ (SCT20) cathodes reveals enhancement of the bulk oxygen ionic-conductivity achieved through co-doping of Nb5+ and Ta5+.", "Our experimental results and density functional theory calculations both show that co-doping results in a favourable balance of oxygen vacancy content, ion mobility and surface electron transfer, which is consistent with the higher performance of the co-doped SCNT cathode at lower temperature.", "Therefore, our highly active perovskite cathode not only presents a simple solution to address sluggish cathode kinetics below 500 °C, but could also provide an effective doping strategy for the design of mixed-conducting materials for SOFC and oxygen-ion transport membrane applications at low temperature.", "Methods Sample syntheses The SCNT material was synthesized through a solid state reaction route by ball milling stoichiometric amounts of SrCO3 (≥99.9%, Aldrich), Co3O4 (≥99.9%, Aldrich), Nb2O5 (≥99.9%, Aldrich) and Ta2O5 (≥99.9%, Aldrich) for 24 h, before pelletizing and sintering the mixture in stagnant air at 1,200 °C for 10 h.", "Subsequently, the sintered pellets were well ground and re-sintered for another 10 h at 1,200 °C.", "SrCo0.9Nb0.1O3−δ (SCN10), SrCo0.8Nb0.2O3−δ (SCN20), SrCo0.9Ta0.1O3−δ (SCT10), SrCo0.8Ta0.2O3−δ (SCT20) and Ba0.5Sr0.5Co0.8Fe0.2O3−δ (BSCF) were also prepared through a similar synthesis route.", "Structure characterization The crystal structures of cathode materials were studied by X-ray powder diffraction and NPD.", "High-resolution NPD data were collected using ECHIDNA, the high-resolution neutron powder diffractometer at the Australian Nuclear Science and Technology Organization (ANSTO)56, with a neutron wavelength of 1.6219(2) Å, determined using the La11B6 NIST standard reference material 660b.", "NPD data were obtained from SCNT within a 6 mm vanadium can for 6 h in the 2θ angular range 4 to 164° with a step size of 0.125°.", "GSAS-II (ref. 57) was employed to perform Rietveld analysis of the high-resolution NPD data, using a cubic perovskite33 starting structure.", "The structure was refined against both the X-ray powder diffraction and NPD data, with atomic displacement parameters for the Co, Nb and Ta, fixed to 0.01.", "High-resolution electron transmission microscopy (HR-TEM, Tecnai F20) in conjunction with selected area electron diffraction was also used for phase identification.", "Conductivity and thermogravimetric analyses A DC 4-probe method was used to measure electrical conductivity of the specimen in flowing air (200 ml min−1).", "The samples for the conductivity measurement were dense bars, which were prepared by pressing the cathode powders followed by sintering at 1,200 °C for 5 h.", "Following this, samples were well milled and polished and silver leads attached as the current and voltage electrodes.", "Electrical conductivity was measured using an Autolab PGSTAT20 work station.", "Ionic conductivities were estimated from oxygen permeability tests carried out by gas chromatography (GC)58.", "Membranes were fabricated by pelletizing cathode powders (milled for 2 h in alcohol at 400 r.p.m.), followed by sintering at 1,200 °C for 10 h and polishing.", "The relative densities of all samples were over 95%.", "Subsequently, the dense pellets were sealed in an alumina tube using silver paste.", "The effective area of the membranes were∼65 mm2 with a thicknesses of 0.07 cm.", "Helium was applied at one side as the sweep gas with a rate of 100 ml min−1 and the other side was exposed to air.", "The overall resistance to oxygen permeation was calculated from the following equation: where R=ideal gas constant F=Faraday constant S=valid area of the membrane =oxygen permeation flux =oxygen partial pressure at the side of membrane exposed to air =oxygen partial pressure at the sweep side It was assumed that bulk ionic conduction dominated the oxygen permeation process because of the relative thickness of the membranes, and therefore Roverall is roughly equal to Rionic.", "Hence, the ionic conductivity of the sample was estimated according the following equation: Where L=the thickness of the membrane.", "The ionic transference (tion) of the samples were calculated using the following equation: Where σtotal and σion are the total electrical and ionic conductivity, respectively.", "Thermal gravimetric analysis was performed by PerkinElmer STA6000 to monitor the mass change of SCNT, SCT20 and SCN20 in flowing air from 200 to 800 °C and also during the abrupt change of atmosphere from flowing air to nitrogen to air at 500 °C.", "Specimens were pelletized and ground using a mortar and pestle to ensure similar grain size before the test.", "Samples were first gradually heated to 200 °C and held for 1 h to remove absorbed moisture.", "The temperature was then increased at a rate of 1 °C min−1 to 500 °C in flowing air (20 ml min−1).", "Subsequently, the flowing gas was abruptly switched to nitrogen, and this condition remained for 2 h until the sample weight stabilized.", "Then, the atmosphere was switched back to air and the mass change recorded until equilibrium was reached.", "The rate of weight change was estimated by: Where mt is the weight of the sample at time t, Δt is the time interval between two recorded adjacent points.", "ORR characterization Cathode polarization resistance was characterized in a cathode|ceria-based electrolyte|cathode symmetrical cell configuration using electrochemical impedance spectroscopy (EIS) carried out with an Autolab PGSTAT20.", "The samples were measured at least three times to ensure accuracy.", "The ceria-based electrolyte was either Sm0.2Ce0.8O1.9 (SDC, from Fuel Cell Materials) or Gd0.1Ce0.9O1.95 (GDC, from Aldrich).", "The symmetrical cells were fabricated by spraying nitrogen-borne cathode slurries onto both sides of SDC dense disks, followed by calcination at 1,000 °C for 2 h in stagnant air.", "Cathode slurries were prepared by suspending powder cathodes in isopropyl alcohol.", "The thicknesses of cathodes were controlled to be around 10 μm, and the active area of each cathode was ∼1.15 cm2.", "SCNT cathodes with different thicknesses were also fabricated by changing the spraying time.", "Silver paste was subsequently painted onto both cathode sides as current collector.", "The symmetrical cell with a silver electrode was fabricated by painting the silver paste onto both sides of the GDC disk, followed by baking at 260 °C for 30 min.", "We evaluated the performance of the LT-SOFC using anode-supported button-like single cells.", "The anode powders were prepared by ball milling the NiO, GDC or SDC, and dextrin (pore former) with a weight ratio of 6:4:1 for 20 h in ethanol.", "The anode-supported single cells were fabricated by drop coating the GDC slurry onto the surface of the anode disks, which were fabricated by pressing anode powders into disks and sintering at 900 °C for 5 h.", "The GDC slurry used in drop coating was prepared by suspending the GDC powders in terpineol and ethanol.", "The coated disks were subsequently sintered at 1,400 °C for 5 h.", "The fuel cell for SDC-based cell stability test was fabricated using co-press method4.", "The cathode fabrication was carried out following similar steps to those for producing the symmetrical cell.", "The mechanisms of the SCNT ORR were studied by fitting the EIS impedance spectra at different pO2 to the Re (R1CPE1) (R2CPE2) equivalent circuit model, where by using the LEVM software.", "The results are presented in (Supplementary Fig. 12) Re represents the ohmic resistance; (R1CPE1) and (R2CPE2) stand for the two ORR steps at high frequency and low frequency respectively.", "The rate determining steps of ORR are indicated by a parameter m given as follows50: Where Rp is the polarization resistance of the corresponding ORR process.", "First-principles calculations First-principles calculations were performed with the Vienna ab initio simulation package (VASP)5960 using density-functional theory.", "Ion-electron interactions were treated using projector-augmented-wave potentials61 and a generalized gradient approximation (GGA) in the form of Perdew–Burke–Ernzerhof was adopted to describe electron–electron interactions62.", "The GGA+U calculations were performed with the simplified spherically averaged approach applied to d electrons, where the coulomb (U) and exchange (J) parameters are combined into the single parameter Ueff (Ueff=U−J), which was set to 0.8 eV in these calculations.", "Electron wave functions were expanded using plane waves with an energy cut-off of 520 eV.", "The Kohn–Sham equation was solved self-consistently with a convergence of 10−5.", "The Brillouin zone was sampled using a 3 × 3 × 3 k-point grid.", "The stoichiometry of the simulated systems was set to SrCo0.75Nb0.25O3, SrCo0.75Ta0.25O3 and SrCo0.75Nb0.125Ta0.125O3, respectively, due to computational limitation, and the Nb and Ta in SCNT are regarded as ordered instead of randomly distributed for simplification.", "The formation energy of an oxygen vacancy was calculated from the energy difference between the total energy of the VO-containing sample and sum of the total energy of pristine sample and the chemical potential of an oxygen atom in an O2 molecule.", "The minimum energy pathway for VO migration was determined using a climbing image nudged band method.", "(CNBE)6364 implemented in the VASP code.", "Data availability The data that support the findings of this study are available from the corresponding authors upon reasonable request.", "Additional information How to cite this article: Li, M. et al.", "A niobium and tantalum co-doped perovskite cathode for solid oxide fuel cells operating below 500 °C.", "Nat.", "Commun. 8, 13990 doi: 10.1038/ncomms13990 (2017).", "Publisher's note: Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations." ]

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[ "Demonstrating the potential of yttrium-doped barium zirconate electrolyte for high-performance fuel cells Demonstrating the potential of yttrium-doped barium zirconate electrolyte for high-performance fuel cells BaeKiho12JangDong Young1ChoiHyung Jong1KimDonghwan12HongJongsup2 http://orcid.org/0000-0001-5959-6871KimByung-Kook2LeeJong-Ho23SonJi-Wona23 http://orcid.org/0000-0002-5310-0633ShimJoon Hyungb1 1School of Mechanical Engineering, Korea University, Anam-ro 145, Seongbuk-gu, Seoul 02841, Republic of Korea 2High-Temperature Energy Materials Research Center, Korea Institute of Science and Technology (KIST), 5, Hwarang-ro 14-gil, Seongbuk-gu, Seoul 02792, Republic of Korea 3Nanomaterials Science and Engineering, Korea University of Science and Technology (UST), KIST Campus, Seoul 02792, Republic of Korea ajwson@kist.re.krbshimm@korea.ac.kr 14553 In reducing the high operating temperatures (≥800 °C) of solid-oxide fuel cells, use of protonic ceramics as an alternative electrolyte material is attractive due to their high conductivity and low activation energy in a low-temperature regime (≤600 °C).", "Among many protonic ceramics, yttrium-doped barium zirconate has attracted attention due to its excellent chemical stability, which is the main issue in protonic-ceramic fuel cells.", "However, poor sinterability of yttrium-doped barium zirconate discourages its fabrication as a thin-film electrolyte and integration on porous anode supports, both of which are essential to achieve high performance.", "Here we fabricate a protonic-ceramic fuel cell using a thin-film-deposited yttrium-doped barium zirconate electrolyte with no impeding grain boundaries owing to the columnar structure tightly integrated with nanogranular cathode and nanoporous anode supports, which to the best of our knowledge exhibits a record high-power output of up to an order of magnitude higher than those of other reported barium zirconate-based fuel cells.", "Protonic ceramic fuel cells are promising for energy applications, but maintaining high performance with long-term stability is an issue.", "Here the authors use a stable yttrium-doped barium zirconate electrolyte, achieving a power output one order of magnitude higher than existing protonic ceramic fuel cells.", "Proton conduction in several doped perovskite oxides has opened new opportunities to use ceramic electrolytes for protonic devices, such as gas sensors, steam electrolyzers, and protonic-ceramic fuel cells (PCFCs)12345.", "Among these, PCFCs have attracted attention because of the possibility of reducing the high operation temperature of conventional ceramic fuel cells (solid-oxide fuel cells, SOFCs, operate at typically 800–1,000 °C) to <600 °C while retaining high ionic conductivity at the low temperatures (LTs) with a significantly low activation energy (<0.5 eV)4567.", "Since the high operating temperature is considered as a main reason for fast degradation and high cost of SOFCs, PCFCs are expected to be a potent alternative to SOFCs.", "In spite of the advantages in LTs, many protonic ceramics (PCs) suffer from poor chemical stability under H2O or CO2 atmosphere, which deteriorates the long-term stability of PCFCs8910.", "In this regard, yttrium-doped barium zirconate (BZY) has been considered as an attractive electrolyte material for PCFCs due to its excellent chemical stability67 as well as high bulk ionic conductivity11121314.", "This excellent chemical stability of BZY against carbon contamination was also confirmed in our preliminary experiments as described in Supplementary Figs 1 and 2.", "However, PCFCs so far developed with BZY electrolytes following the conventional fabrication process of SOFCs have demonstrated unsatisfactory performance (blue box in Fig. 1).", "The reported poor performance of BZY-PCFCs is mainly due to the high ohmic resistance of the electrolyte.", "One probable contributor is the highly resistive grain boundaries of BZY in proton conduction, resulting in large ohmic resistance and low-power outputs of the PCFC1516.", "Hence, minimization or ideally elimination of the grain boundaries in the electrolytes can be beneficial during the cell fabrication of BZY-PCFCs to achieve high performance at LTs.", "However, poor sinterability of the BZY material requiring for a high sintering temperature (∼1,700 °C) for sufficient grain growth1718 has discouraged successful synthesis of highly conductive dense thin-film BZY membrane.", "As a way to promote grain growth of BZY without high sintering temperature, the addition of sintering aids have been suggested1920, but the consequent conductivity reduction nullifies the merit of using BZY for replacing conventional oxygen-ion-conducting oxides.", "Solid-state reactive sintering, where material synthesis and sintering are carried out simultaneously using nano-size precursors, has enabled the growth of relatively large BZY grains and effectively reduced grain-boundary resistance1421.", "However, a fuel cell having a BZY electrolyte with such large grain sizes (∼1 μm) has not been reported yet to the best of our knowledge.", "The most straightforward approach to lowering the ohmic resistance of the BZY electrolyte is to reduce its thickness while eliminating the impeding grain boundaries.", "There have been recent successes in high-conductivity measurements from thin-film-deposited BZY1213141516171819202122, confirming that fabrication of a highly conductive BZY electrolyte is possible as long as one retains the reduced thickness as well as no grain boundaries.", "Indeed, PCFCs with thin-film BZY electrolytes have been successfully developed using the free-standing membrane-electrode assemblies (MEAs), and demonstrated reasonably high-power outputs at the reduced temperatures below 450 °C (green box in Fig. 1).", "However, poor mechanical stability and limited effective areas of the free-standing MEA-based PCFCs prevent those to function as a practical device2324.", "Here we propose use of a ‘multi-scale' anode to grow thin and dense BZY membrane atop, and report the successful fabrication of a well-integrated BZY electrolyte with columnar-grain-structure being free of grain-boundary across the film.", "As a result, our fuel cells have marked the topmost fuel cell performance among those of the reported BZY-based PCFCs (red data points in Fig. 1).", "We expect that our approach may provide a potential framework to develop highly-performing PCFCs working at LTs.", "Results Thin-film BZY PCFC with multi-scale anode structure To achieve the desired structural characteristics of the BZY membrane, that is, a thin thickness and columnar microstructure while keeping the gas tightness, in the anode-supported cell configuration, the surface condition of the anode is crucial.", "In the case of free-standing PCFCs, fabrication of impermeable ultra-thin BZY electrolytes with thicknesses of ∼100 nm was possible, because the perfectly flat and dense surfaces were provided for the thin-film deposition by the underlying substrates, single-crystal silicon (Si) wafers2526.", "However, depositing a thin and dense electrolyte over powder-processed anode supports with micron-scale pores is substantially challenging27, because pinholes are generated due to the selective nucleation of the film at the edges of pores28 and incomplete coverage of the electrolyte layer is inevitable.", "Hence, an optimal anode structure with high-quality surface suitable to thin-film deposition is essentially required to realize high-performance thin BZY electrolyte-based PCFCs.", "In this regard, multi-scale anode structure is proposed in the work, as presented in Fig. 2.", "The multi-scale anode structure contains nanostructure anode surface layer (nano anode functional layer, nano-AFL) over the conventional powder-processed anode body consisting of an AFL with micron-size grains (micron-AFL) and anode support.", "The nano-AFL is formed by the thin film deposition, in this case by pulsed laser deposition (PLD).", "The insertion of the nano-AFL on porous electrode supports has significantly improved the integrity of the thin electrolyte and enhanced fuel cell performances in SOFCs2930313233.", "The main reasons for the improvement are (i) reduced number of defects and roughness of the anode surface, which is preferable for dense electrolyte film growth2830; (ii) increased the triple phase boundary length with smaller electrode grains31323334; and (iii) reduced interfacial resistances with more contact area between the electrolyte and the electrode3335.", "To obtain fully integrated and reproducible microstructure of PCFCs based on thin BZY electrolytes, however, is much more difficult in comparison with the cases of SOFCs, because the poor sinterability of BZY also affects the properties of the deposited films.", "The poor sinterability of BZY leads to retarded densification in thin-film deposited and post-annealed NiO–BZY and poor interface adhesion with the anode support.", "Through a meticulous optimization of the multi-scale anode fabrication, we succeeded in obtaining a structurally stable and thin BZY electrolyte, as presented in the scanning electron microscopy (SEM) images in Fig. 2.", "More details of microstructure of the optimized PCFC are in Supplementary Fig. 3.", "Highly dense BZY electrolyte with a composition of BaZr0.85Y0.15O3−δ deposited on multi-scale Ni–BZY anode with different grain and pore sizes are clearly observed.", "Discussion of the optimization process will be followed in the next session.", "Optimization of the BZY-PCFC fabrication The surface layer of the NiO–BZY anode support, micron-AFL, is formed by the tape casting, and sintered at high temperature of 1,450 °C.", "Due to this high-temperature sintering, the surface roughness of the micron-AFL aggravates due to the protrusion of overly grown NiO grains exhibiting BZY grain size of ∼0.5 μm or less and NiO grain size of ∼2 μm in the sintered body.", "Therefore, brief surface grinding was carried out and surface morphology of the micron-AFL after that is shown in Fig. 3a.", "After reduction of micron-scale NiO to Ni, micron-size pores are generated in micron-AFL, as shown in Fig. 3b.", "The large pore generation causes huge stress at the interface between anode and electrolyte and damages physical stability of the thin electrolyte floating over the pores.", "To find an optimal surface morphology of the anode to sustain the thin BZY electrolyte, numerous microstructural factors, such as the grain and pore sizes, density of the surface after the post annealing, suppression of the Ni agglomeration and pore generation while the reduction, are considered for the fabrication of NiO–BZY nano-AFL.", "Ni content and post-annealing temperature of nano-AFL are identified as key factors to determine the microstructural factors.", "From the optimization, it was concluded that the most satisfactory quality of nano-AFL is obtained when the nano-AFL contains 50 vol% Ni and is post annealed at 1,300 °C.", "Detailed discussion on the optimization of the nano-AFL is in the Supplementary Materials.", "By applying optimized NiO–BZY nano-AFL over the micron-AFL, the surface of the anode is now covered with grains with diameter ∼100 nm (Fig. 3c) and the size of open pores is also much reduced in comparison with that of the micron-AFL after the anode reduction (Fig. 3d).", "The impacts of the anode optimization, particularly focusing on nano-AFL, are clearly compared in Fig. 4.", "The open-circuit voltage (OCV) profiles in Fig. 4a were obtained from two different PCFCs during the anode reduction with varying H2 concentration from 0 to 100% in N2 valance.", "The first PCFC adopted nano-AFL fabricated under the optimal condition (50 vol% Ni and is post annealed at 1,300 °C) and the second PCFC used a non-optimized condition, with a 100 °C lower post-annealing temperature.", "An irreversible OCV drop appears in the PCFC fabricated under the non-optimized conditions, whereas the OCV of the optimized PCFC sharply increased after the 80% H2 reduction step.", "Only the optimized PCFC eventually reached high OCVs close to the theoretical value of BZY considering the transference number combined the electric and ionic transports (∼1.08 V at 600 °C)11.", "To check the reproducibility of the OCV values, at least three PCFCs fabricated at the identical condition were tested in the optimization process (Fig. 4 and Supplementary Fig. 6).", "As the result, high OCVs with small scatter were obtained from the optimal PCFCs, indicating that the thin and dense BZY electrolytes can be reproducibly fabricated on the optimized anode structure.", "In contrast, the PCFCs with non-optimized nano-AFLs always yielded poor OCVs.", "The reason of this difference between the two types of PCFCs is revealed from post-mortem SEM observation (Fig. 4c,d).", "The cross-sectional SEM images of the non-optimized PCFC show delamination between nano- and micron-AFLs (Fig. 4c), indicating the poor adhesion of the nano-AFL and the powder-processed anode surface.", "This delamination is expected to accompany local cracks through the membrane, resulting in the abrupt OCV drop with crossover of hydrogen during the reduction step shown in Fig. 4a.", "It appears that the annealing temperature of 1,200 °C is insufficient to develop interfacial adhesion by connecting BZY grains between nano- and micron-AFLs due to the poor sinterability of BZY.", "On the other hand, good interfacial adhesion was observed in the cross-section SEM images of the optimal PCFC, which would ensure both ionic and electronic paths through the entire anode (Fig. 4d).", "It should be noted that high OCV was observed in the optimized cell at high concentration of hydrogen (Fig. 4a).", "We suspect that this is due to the structural characteristics of nano-AFLs, which comprises multiple layers with well-ordered nano-size pores, as shown in Fig. 4d.", "This nanoporous structure is favourable for sustaining thin and dense BZY electrolytes and for promoting the charge-transfer reaction at electrolyte–electrode boundaries.", "However, it is also anticipated that getting effective gas supply thoroughly through the layers could be challenging through such small pores.", "Therefore, opening up these small pores by reduction throughout the nano-AFLs could be retarded significantly, especially when low-concentration hydrogen is used.", "Moreover, the supply gas should compete against the counterflow of the water outgas that is a product of NiO reduction, which implies that hydrogen delivered near the electrolyte could be diluted more.", "In the case of non-optimized nano-AFLs, however, relatively large-scale cracks or spaces between the delaminated layers form, as shown in Fig. 4c, where the hydrogen supply gas could be delivered more effectively through these large spaces and thus competition against counterflow water outgas should be less severe.", "For this reason, OCV of the non-optimized PCFC appeared at a relatively early stage with a relatively low concentration of hydrogen, as observed in Fig. 4a.", "Microstructural characteristics of the optimized PCFC Figure 5a shows a schematic of a single columnar grain in the thin BZY electrolyte and a LSC (La0.6Sr0.4CoO3−δ) cathode and a Ni–BZY anode contacting each side of the BZY column.", "The schematic is drawn based on the transmission electron microscopy (TEM) analyses shown in Fig. 5b–f.", "First, highly dense BZY electrolyte is observed in the bright-field TEM image in Fig. 5b.", "In Fig. 5b, nano-porous LSC and Ni–BZY layers are also shown as top and bottom layers, respectively.", "The dense or porous structures of the each layer are more clearly shown in the images of a higher magnification (Fig. 5c).", "In the dark-field TEM image (Fig. 5d), it is confirmed that the columnar structure of the BZY electrolyte is a single grain, which does not have grain boundaries impeding the proton transfer path from the anode to the cathode.", "The selected area electron diffraction (SAED, obtained from the marked area in Fig. 5b) revealed that the BZY electrolyte is fully crystallized, single-phase cubic perovskite BZY (Fig. 5e).", "From the high-resolution-TEM (HR-TEM) image in Fig. 5f the lattice spacing of 0.29 nm can be obtained and it is in a good agreement with the (110) plane spacing of BZY3637.", "The X-ray diffraction and SEM-energy dispersive X-ray spectroscopy (EDS) measurement of the BZY electrolyte fabricated using the same PLD conditions on sapphire substrates have confirmed that the stoichiometry matched well to that of one of the PLD targets with no secondary phase, as represented in Supplementary Fig. 8.", "The high proton conduction in BZY single grain (bulk) has been identified in many studies, superior to those of the other protonic ceramics11141738.", "In recent, the exceptionally high conductivity from the epitaxial BZY thin films grown on MgO single-crystal substrates121322 raised the expectation to obtain highly performing BZY-based PCFCs by extremely limiting the numbers of the impeding grain boundaries.", "Until now, however, it has been extremely challenging to eliminate the grain boundaries encountering the current flow direction in the full cell, both by the powder processing and thin-film deposition.", "For the former, the electrolytes with very small grains and thus very high grain-boundary density are generally obtained because of the poor sinterability of BZY, and for the latter, it has been nearly impossible to deposit gas-impermeable thin BZY electrolyte over the porous anode support.", "Therefore, the results shown in Fig. 5 have significant importance, because these demonstrate that it is possible to realize the grain-boundary-free BZY electrolyte in the direction of proton transport by using a thin-film deposition technique and by adopting the multi-scale anode structure.", "Moreover, the nano-sized electrode grains are expected to improve the performance, providing sufficient electrode reaction sites on the both sides of the electrolyte.", "Electrochemical characteristics of the optimized PCFC The electrochemical performances of the BZY PCFC fabricated under the optimal conditions are depicted in Fig. 6a–d.", "In Fig. 6a, a drop in the voltage at a low current is observed at <500 °C, whereas a fall curve at a higher current is observed at 600 °C.", "This is because the electrode response is limited to other factors at different temperatures.", "Specifically, charge transfer reactions are considered to dominate overall electrode kinetics at low temperatures.", "A temperature increase to 600 °C is expected to help improve the rate of electrochemical reactions and mass diffusion can dominate the electrode process because the reactants can still undergo transfer through small pores present in the nano-AFL.", "The power output reached a maximum of 740 mW cm–2 at 600 °C along with values of 563, 457 and 342 mW cm–2 at the other temperatures of 550, 500 and 450 °C (Fig. 6a).", "This power achievement is enhanced significantly compared with data from previously studied BZY-based cells, confirmed in Fig. 1 and supplementary Table 1, and greater than record data from all PCFCs previously developed (650 mW cm–2 at 600 °C)39.", "The OCV values were about 1.0 V, which can be considered to be in a reasonable range compared to that of the previously reported BZY-based PCFC4041424344454647, especially considering the low thickness of the electrolyte.", "It implies that the thin BZY electrolyte has the appropriate structural integrity to function as an electrolyte.", "However, the OCV is rather insensitive to temperature change, which may originate from certain leakage issues such as sealing.", "The performance improvement attributes to the results of the well-designed fuel cell configuration and its optimization as previously discussed above.", "Figure 6b presents AC impedance spectra obtained at each temperature under OCV condition.", "Due to the complexity and many processes involved in the whole fuel cell reactions, subdivided interpretation is difficult from the impedance data, but ohmic and polarization resistances were able to be estimated.", "The intersection points with x axis at the high- and low-frequency regime were used for the ohmic and polarization area-specific resistances (ASRs), respectively.", "To examine the significant improvement of electrochemical performance, the ohmic and polarization ASRs of representative BZY-PCFCs found in the literature were compared (Fig. 6c,d).", "An order of magnitude lower ohmic ASRs were achieved in the current work compared to the reference values, as shown in Fig. 6c.", "These results suggest that the significantly reduced thickness of the BZY electrolyte is the main cause of the improved cell performance.", "The improvement in bonding between the porous anode and the thin and dense columnar BZY layer, as shown in Fig. 5, also seems to have contributed to the reduction in ohmic ASRs.", "Relatively low-polarization ASRs were also observed during the comparison (Fig. 6d).", "We believe that the nano-size grains of the LSC cathode and the Ni-BZY nano-AFL increased the number of active sites in the electrode reaction.", "Further improvement is expected by use of a high-performing and stable cathode material substituting for the LSC that has negligible proton conductivity48.", "Moreover, the improved integration of electrolyte and anode support by adoption of the multilayered AFLs using multistep post-annealing has been observed clearly in the cross section of the stack, as presented in Figs 4d and 5, which is considered to have contributed significantly to the improved charge-transfer reaction, decreased polarization ASRs and enhanced fuel cell power.", "Discussion To fabricate highly efficient and physically/chemically stable PCFCs, an anode-supported fuel cell configuration based on BZY thin films is demonstrated in the current study.", "The multi-scale anode structure with reducing grain and pore sizes is confirmed to provide flat surface favourable to thin-film deposition as well as improve physical integration.", "On the anodes, a grain-boundary-free columnar BZY electrolyte with significantly reduced thickness was successfully fabricated by PLD.", "This thin BZY electrolyte is believed to substantially reduce the ohmic resistance compared with those of BZY-PCFCs quoted in literature, which is the main reason for the cell performance enhancement.", "The nano-porous electrodes clearly shown by TEM images were also sufficient to implement low-polarization resistance, providing increasing reaction sites on the both side of the electrolyte.", "As results, significantly improved power outputs were obtained from the fuel cell configuration with the maximum power density of 740 mW cm−2 at 600 °C that has not achieved from the other BZY-based PCFCs so far.", "This performance improvement using BZY provides an opportunity for practical use of PCFCs potentially solving the conflicting challenges between high performance and chemical stability that have been faced in PCFCs until now.", "Methods Preparation of PCFCs with thin-film BZY electrolytes Tape-casted NiO–BZY composites (a Ni:BZY volume ratio of 40:60 in the solid content after reduction; composition of the anode BZY powder: BaZr0.85Y0.15O3−δ) were sintered at 1,450 °C for 10 h in air and used as the anode support.", "Micron-AFL tape sheet (10 μm in thickness) was placed on the porous anode body tapes containing 30 vol% polymethyl methacrylate pore formers and laminated with a cell size of 1 × 1 cm2.", "After the sintering of the anode support, surface grinding was treated to remove the NiO particles protruded from the sintered surface.", "Then, nano-AFLs (∼3 μm in thickness) were deposited by PLD with a 50 vol% Ni containing NiO–BZY target.", "A KrF excimer laser (λ=248 nm, Compex Pro 201 F, Coherent) was used as the ablation source with a laser fluence of ∼2.5 J cm−2 and a repetition rate of 10 Hz.", "The substrate temperature, O2 background pressure, and target-to-substrate distance were kept at 750 °C, 6.67 Pa, and 5 cm, respectively, during the deposition.", "The nano-AFLs were post annealed in ambient air at 1,300 °C for 1 h with a uniform heating and cooling rate of 2 °C min−1.", "Dense BZY electrolyte layers (2.5 μm in thickness) were deposited under the same PLD conditions used for nano-AFLs.", "Validity of this process for growing BZY films is discussed rigorously and confirmed in our previous work49.", "The deposited BZY electrolytes were followed by annealing at 1,200 °C for 3 h to improve adhesion at the interface with the anode support.", "Porous LSC (2 μm in thickness) was deposited as the cathode by PLD at room temperature with an O2 pressure of 13.3 Pa and an area of 0.3 × 0.3 cm2.", "This process was followed by annealing at 650 °C for 1 h to form a porous morphology.", "Fuel cell test Before operating the fuel cell, reduction of the anode was performed by gradually increasing the H2 concentration from 0 to 100% with N2 as the balance gas at 600 °C for 9 h while measuring the OCVs every 10 s.", "Humidified H2 gas (3% H2O) was flowed on the anode side at 50 ml min−1, and air was fed as the oxidant on the cathode side at the same flow rate during the test.", "An Au mesh and Ni foam were placed on the cathode and anode surfaces, respectively, for current collection, and a commercial alumina paste (P-24, Toku Ceramic) was used for gas sealing.", "The I–V and AC impedance data were collected at 450–600 °C using the Gamry framework system (Gamry Reference 3000 Potentiostat/Galvanostat/ZRA).", "The impedance data were obtained in the frequency range of 106–0.1 Hz with an amplitude of 10 mV under OCV condition.", "The data were analysed using Z-view software (v3.4c, Scribner Associate Inc.).", "Microstructure observation The prepared anode supports or NiO–BZY nano-AFLs deposited on them were placed in a tube furnace under the flow of 4% H2–Ar at 650 °C for 10 h to investigate the morphology changes of nano-AFLs resulting from reduction.", "SEM (XL-30 FEG, FEI) was utilized to observe morphologies of the anode surface and the full cell surface and cross-section.", "To investigate in-depth microstructure crystallinity of the thin BZY electrolyte and its near anode and cathode grains, TEM (Tecnai F20, FEI) was used.", "Focused ion beam (Helios NanoLab 600, FEI) was used to prepare the TEM sample.", "Data availability The authors declare that the main data supporting the findings of this study are available within the article and its Supplementary Information files.", "Extra data are available from the corresponding author upon request.", "Additional information How to cite this article: Bae, K. et al.", "Demonstrating the potential of yttrium-doped barium zirconate electrolyte for high-performance fuel cells.", "Nat.", "Commun. 8, 14553 doi: 10.1038/ncomms14553 (2017).", "Publisher's note: Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations." ]

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[ "Roles of Bulk and Surface Chemistry in the Oxygen Exchange Kinetics and Related Properties of Mixed Conducting Perovskite Oxide Electrodes Roles of Bulk and Surface Chemistry in the Oxygen Exchange Kinetics and Related Properties of Mixed Conducting Perovskite Oxide Electrodes PerryNicola H.", "*IshiharaTatsumi MenzlerNorbert H.", "Academic Editor International Institute for Carbon-Neutral Energy Research, Kyushu University, 744 Motooka, Nishi-ku Fukuoka 819-0395, Japan; ishihara@cstf.kyushu-u.ac.jp *Correspondence: perry@i2cner.kyushu-u.ac.jp; Tel.: +81-092-802-6739 858 Mixed conducting perovskite oxides and related structures serving as electrodes for electrochemical oxygen incorporation and evolution in solid oxide fuel and electrolysis cells, respectively, play a significant role in determining the cell efficiency and lifetime.", "Desired improvements in catalytic activity for rapid surface oxygen exchange, fast bulk transport (electronic and ionic), and thermo-chemo-mechanical stability of oxygen electrodes will require increased understanding of the impact of both bulk and surface chemistry on these properties.", "This review highlights selected work at the International Institute for Carbon-Neutral Energy Research (I2CNER), Kyushu University, set in the context of work in the broader community, aiming to characterize and understand relationships between bulk and surface composition and oxygen electrode performance.", "Insights into aspects of bulk point defect chemistry, electronic structure, crystal structure, and cation choice that impact carrier concentrations and mobilities, surface exchange kinetics, and chemical expansion coefficients are emerging.", "At the same time, an understanding of the relationship between bulk and surface chemistry is being developed that may assist design of electrodes with more robust surface chemistries, e.g., impurity tolerance or limited surface segregation.", "Ion scattering techniques (e.g., secondary ion mass spectrometry, SIMS, or low energy ion scattering spectroscopy, LEIS) with high surface sensitivity and increasing lateral resolution are proving useful for measuring surface exchange kinetics, diffusivity, and corresponding outer monolayer chemistry of electrodes exposed to typical operating conditions.", "Beyond consideration of chemical composition, the use of strain and/or a high density of active interfaces also show promise for enhancing performance. solid oxide fuel cell (SOFC) solid oxide electrolysis cell (SOEC) perovskite oxygen exchange defect chemistry conductivity chemical expansion surface chemistry segregation strain 1.", "Introduction: Solid Oxide Fuel and Electrolysis Cells Fuel cells directly convert the chemical energy of fuel and oxygen to electrical power with potential for significantly higher efficiency than conventional heat engines [1,2,3,4,5].", "Among the various types of fuel cells, solid oxide fuel cells (SOFCs), using oxide ion (or proton) conducting ceramic electrolytes, operate at high temperatures (around 873–1273 K), thus providing the ability to directly use a variety of hydrocarbon fuels with high fuel-to-electricity conversion efficiency (>55%, lower heating value (LHV)) [2].", "Moreover, when the waste heat is utilized, in combined heat and power (CHP) applications, they can exceed 85% efficiency [6], unmatched by any other energy conversion technology.", "Therefore, SOFCs are now attracting much interest for power generation.", "Components of SOFCs include the cathode (oxygen electrode), anode (fuel electrode), and ionically conducting electrolyte between them; see Figure 1a.", "Individual SOFC cells are electrically connected in series by interconnects, leaving space for gas channels, to create an SOFC “stack” [1,2,3,4,5]; parallel connection of cells may also be incorporated for stack lifetime considerations.", "For several decades, Y2O3 stabilized ZrO2 (YSZ) has been the workhorse SOFC electrolyte, because of its reasonably high ionic conductivity, very low electronic conductivity, low cost, and mechanical strength [1,2,3].", "Owing to YSZ’s limited ionic conductivity, early SOFCs operated at ~1273 K.", "While such high temperatures can boost the thermally-activated oxide ion transport, they also result in high cell costs, long start-up and shut down cycles, and unacceptable performance degradation rates.", "Therefore, at present, improvement in long term stability is an important issue for SOFC development.", "Contributing factors to power density degradation in SOFCs [7] include (1) poisoning of the electrodes by chemical impurities such as S or Cr; (2) reactions between components; (3) sintering or aggregation; and (4) delamination.", "Degradation modes specific to the oxygen electrode are discussed in more detail later, but for all of these factors, clarifying the mechanisms and driving forces is a subject of ongoing research [8,9,10,11].", "On the other hand, recently, there has also been strong interest in reversible operation of SOFCs, i.e., as “Solid Oxide Electrolysis Cells (SOECs)” from an energy storage point of view.", "Since the use of renewable energy, such as wind or solar power, is increasing, the generated electrical power may not match demand, because the renewable electric power supply fluctuates.", "In order to store and average electric power, electrolysis of water into chemical fuel is now attracting interest.", "There are several types of electrolysis cell, including alkaline, polymer, and high temperature ceramic cells.", "Here, conversion efficiency from electricity to hydrogen is also important.", "The conversion efficiency increases in the following order: alkaline (ca. 70%) < polymer (ca. 80%) < high temperature (ca. 90%).", "In high temperature electrolysis, the Gibbs free energy required for the water splitting reaction, which corresponds to the required applied voltage, decreases with increasing temperature because of the increased heat energy (TdS).", "Therefore, extremely high efficiency can be achieved in high temperature electrolysis.", "However, there are still many issues to address for SOECs; in particular, degradation of the cell is more significant compared with SOFCs.", "At present, the materials used for SOECs are similar to those of SOFCs; however, compared with SOFCs, greater tolerance for severe oxidation and tight gas sealing are required [12,13].", "For both types of cell, oxygen electrodes play a highly important role in determining efficiency, and superior catalytic activity, transport properties, and stability are required.", "In this non-exhaustive review, the role and fundamental properties required of oxygen electrode materials in SOFC and SOEC modes are explained, examples of oxygen electrode chemistries are given, and then investigations into the impact of both bulk and surface chemistry (such as surface segregation) in determining performance and degradation are summarized.", "The paper primarily focuses on some of the work in progress in this field within the International Institute for Carbon-Neutral Energy Research (WPI-I2CNER) at Kyushu University, and additionally, selected work from the broader community is discussed and highlighted. 2.", "Role and Required Properties of Oxygen Electrodes Oxygen electrodes for solid oxide fuel/electrolysis cells (SOFCs/SOECs) mediate the electrochemical reduction of gaseous oxygen into oxide ions (SOFC cathode) or oxidation of oxide ions into gaseous oxygen (SOEC anode), respectively, at elevated temperatures (typically 873–1273 K).", "The former process, the oxygen reduction reaction (ORR) at the cathode of SOFCs, is given below in Kroger-Vink (point defect) notation, where the main symbol indicates the species (O = oxygen, e = electron, V = vacancy, and h = hole), superscript indicates the relative charge (′ = negative, × = neutral, · = positive) and subscript indicates lattice site (O = oxygen site, i = interstitial site).", "The ORR reaction can be written: (1) 1 2 O 2 ( g ) + 2 e ′ + V O ⋅ ⋅ → O O × or 1 2 O 2 ( g ) + V O ⋅ ⋅ → O O × + 2 h ⋅ if the electrode conducts oxide ions by an oxygen vacancy mechanism, and (2) 1 2 O 2 ( g ) + 2 e ′ + V i × → O i ′′ or 1 2 O 2 ( g ) + V i × → O i ′′ + 2 h ⋅ if the electrode conducts oxide ions by an oxygen interstitial mechanism.", "The former process would be typical of oxygen sub-stoichiometric perovskites with formula ABO3−δ, whereas the latter process would be more typical of oxygen super-stoichiometric Ruddlesden-Popper phases A2BO4+δ, for example.", "(Often A = La, Sr, Ca, or Ba and the B site is at least partially occupied by a multivalent cation, such as Ni, Fe, Co, Mn, or Cr) The oxygen evolution reaction (OER), taking place at the anode of SOECs, is essentially the reverse reaction.", "As these reactions involve gaseous oxygen, electronic charges, and oxide ions, the oxygen electrode should ideally be capable of transporting all of these species.", "Sometimes this reaction occurs locally at “triple phase boundaries (TPBs)”, where a gas channel (or pore), an electronic conducting phase, and an oxide ion conducting phase contact each other, for example in composite electrodes or in purely electronically conducting electrodes at the interface with the ionically conducting electrolyte.", "On the other hand, in many mixed ionic and electronic conducting (MIEC) materials, i.e., oxides that can conduct both electronic species and oxygen vacancies or interstitials within their lattice, the reaction may take place over the full surface area of the electrode, depending on the availability of charge carriers.", "Figure 1b illustrates these different pathways for the ORR [14]—the “bulk pathway” incorporating oxygen over the full electrode surface, and the “surface pathway” where oxygen first diffuses and then reacts at a TPB, the electrode/ electrolyte/gas phase interface.", "When the “bulk pathway” is operating, fast bulk chemical diffusion is also essential for efficient transport of oxide ions between the electrode surface and the electrolyte; this factor becomes more important for thicker electrodes and is considered performance-limiting for electrodes with thicknesses significantly above the “critical length”, Lc = k/D, where k is the (temperature- and oxygen partial pressure (pO2)-dependent) surface exchange coefficient, and D is the (temperature- and pO2-dependent) diffusivity.", "Alternatively for very thin (or nanostructured, high surface area) electrodes well below the critical length, and often at lower temperatures, the surface exchange process becomes performance-limiting.", "Therefore, in addition to these transport requirements, the electrode surface must possess catalytic activity to enable the various steps of the surface ORR/OER reactions, such as adsorption/desorption, dissociation/association, charge transfer, and lattice incorporation/excorporation, to progress with low activation energies, and to give a high overall value of k.", "For practical long-term operation, the electrodes should maintain both high D and k for long periods of time (several years), including start/stop cycles; values of tracer diffusivity, D* ≥ 10−6 cm2/s and tracer surface exchange coefficient, k* ≥ 10−4 cm/s have been suggested [15].", "Therefore one final requirement for electrode materials is thermo-chemo-mechanical stability over the range of operating conditions.", "While higher temperatures are beneficial for enhancing the thermally-activated surface exchange and diffusion processes, the kinetics of performance degradation processes may also be increased at higher temperatures where ions are more mobile.", "(On the other hand, thermodynamic driving forces for degradation processes may not share this activated temperature dependence).", "Potential instabilities may arise from: decomposition, ordering, or crystal structure changes of the electrode phase itself if it is metastable in the operating conditions; reactions between composite electrode phases or between electrodes and other cell components; changes in surface chemistry arising from intrinsic surface segregation, extrinsic surface poisoning, or a combination of both; microstructural coarsening; delamination from the electrolyte in SOEC mode when high oxygen chemical potentials occur; and stresses arising from thermal and/or chemical expansion.", "The latter effect is particular to materials that can change stoichiometry during operation, typically oxygen loss/gain, resulting in localized lattice distortions and macroscopic strain [16]; the corresponding chemical stresses may exceed the strength of the brittle ceramic components [17] and cause mechanical damage [18].", "In the case of SOECs, the function of the oxygen electrode is opposite to that of the SOFC cathode, i.e., combination of oxide ions to form gaseous oxygen molecules (reverse of Equations (1) and (2)).", "Therefore, the high oxygen pressures experienced by the electrode in this mode can lead to unique degradation mechanisms at the oxygen electrode-electrolyte interface, such as chemical strains owing to changes in lattice defect chemistry at high oxygen pressures (e.g., cation vacancies, oxygen interstitials), grain boundary fracture, formation of secondary phases, and delamination [19].", "Degradation modes for oxygen electrodes are illustrated in Figure 2.", "In this review, the roles of bulk and surface chemistry in impacting the aforementioned electrode properties, particularly the oxygen surface exchange process, will be discussed.", "The review is limited to oxide ion, rather than proton, conducting electrodes, and focuses on perovskite and perovskite-related structures. 3.", "Example Electrode Chemistries Traditionally, perovskite-structured oxides (ABO3) have been considered the most suitable materials satisfying these requirements for oxygen electrodes, and LaFeO3, LaCoO3, or LaMnO3 doped with Sr or Ca have been widely used.", "In the early stages of SOFC development, La0.8Ca0.2MnO3 or La0.6Sr0.4MnO3 oxygen electrodes were commonplace; however, because of the low oxide ion conductivity in Mn-based perovskites, the ORR/OER reaction is typically (though not exclusively [20]) limited to the TPB shown in Figure 1, resulting in large cathodic overpotentials (SOFC mode).", "However, several more complex perovskite oxides have been reported to show very high oxygen surface exchange rates.", "Baumann et al. [21] compared several Co- and Fe-based perovskites with controlled geometries/morphologies, finding that Ba0.5Sr0.5Co0.8Fe0.2O3−δ (BSCF) shows 100 times smaller electrochemical resistance than that of La0.6Sr0.4Co0.2Fe0.8O3−δ (LSCF), which is often used for intermediate temperature SOFC cathodes.", "One reason for such high cathodic activity is the high mixed conductivity, enabling a large reaction area to be available for oxygen incorporation, i.e., the two phase boundary route (“bulk pathway”) in Figure 1.", "Another highly active oxygen electrode composition is Sm0.5Sr0.5CoO3−δ which also demonstrates high oxide ion conductivity [22].", "However, the most popular composition used for SOFC cathodes still remains La0.6Sr0.4Co0.2Fe0.8O3−δ (LSCF), for the reasons of high surface activity, good mixed conductivity, high stability, and moderate cost.", "Recently, research has shifted to perovskite-related structures such as double perovskites (A2B2O6−δ) and layered Ruddlesden-Popper compounds (An+1BnO3n+1), e.g., n = 1 K2NiF4-related structures.", "Examples of double perovskites reported to exhibit promising oxygen electrode properties include ABaCo2O6−δ (A = Nd, Pr, Sm, Gd) [23,24,25] and Ba2Co2−xBxO6−δ (B = Sc, Bi) [26], and so not only perovskites but also perovskite-related phases, in particular, highly oxygen deficient perovskite phases, are now attracting much attention as the active oxygen electrode materials for intermediate temperature operation.", "Beyond changing the crystal structure, increasing the mixed conductivity, and increasing the oxygen deficiency, another strategy to improve oxygen electrode performance is nanostructural engineering.", "Making use of highly active interfaces between phases or within the same phase is one approach; for example Sase et al. [27] reported that the presence of the (La,Sr)2CoO4 phase on (La,Sr)CoO3 electrodes enhances the oxygen exchange reaction rate, and Yildiz et al. [28,29] have proposed explanations for the enhanced ORR activity at the interface between these phases.", "More recently, grain boundaries in the predominantly electronically conducting LSM have been demonstrated to be active paths for oxygen incorporation, with higher k* and D* than in the grains [30].", "Using techniques such as pulsed laser deposition (PLD), it is possible to create thin film electrodes with controlled nano-architectures, exhibiting a high density of interfaces parallel to the direction of oxygen incorporation.", "In Figure 3, one example of such an approach, named a “double columnar system” or sometimes “vertically aligned nanostructure (VAN)”, is shown schematically [31].", "In this structure, nano-sized columns of Sm doped CeO2 and Sm0.6Sr0.4CoO3 have been deposited by the PLD method.", "High resolution transmission electron microscope (TEM) images of the prepared “double columnar system” are shown in Figure 3b,c, where it can be clearly seen that a columnar structure consisting of two different compositions was successfully deposited on the electrolyte substrate.", "Figure 4 shows the power generation ability of a SOFC single cell with and without a double columnar interlayer between the electrolyte and porous oxygen electrode [31].", "In this cell, a Ni-Fe metallic anode substrate, Sm doped CeO2 buffer layer, La0.9Sr0.1Ga0.8Mg0.2O3 (LSGM) oxide electrolyte (500 μm thickness), and porous Sm0.5Sr0.5CoO3 electrode were used.", "Although the double columnar layer is nominally dense (i.e., does not presumably have a high surface area), the observed open circuit potential is close to the theoretical one (1.10 V) suggesting its reasonable activity for the ORR process.", "Obviously, because of the thin LSGM electrolyte film, a high power density close to 2 W/cm2 at 973 K is achieved.", "By comparing the performance of the two cells, it is clear that the power density is increased by using a double columnar structured cathode interlayer.", "A detailed analysis of the internal resistance suggests that the increased power density can be assigned to the decreased cathodic overpotential.", "Therefore, control of nano-structure within the oxygen electrode, in this case the increase in two phase boundary area between the mixed conductor and the ionic conductor, can be important for tailoring the ORR/OER activity. 4.", "Role of Bulk Chemistry With the ultimate goal of optimizing electrode performance by tailoring its chemistry, much work has focused on trying to elucidate relationships between overall (bulk) electrode chemistry, defect chemistry, electronic structure, and electrode properties.", "Ultimately such descriptors could enable rational design and high throughput search and discovery of superior electrode chemistries.", "Nonetheless, since many properties must be simultaneously satisfied, and there are usually trade-offs involved, the “ideal” electrode chemistry may depend on particular requirements of an application.", "Point defect chemistry of bulk electrodes can be inferred from fitting thermogravimetric measurements of oxygen content [32], electrical conductivities [33,34], and/or lattice parameters [35] as a function of temperature and oxygen partial pressure with interrelated mass action expressions of defect generating equations.", "In thin film electrodes, additional techniques include chemical capacitance and optical absorption measurements [36], which can both indirectly provide information about oxygen content. 4.1.", "Bulk Chemistry Impact on Transport Oxide ion conductivity, in general, requires both oxygen non-stoichiometry to provide charge carriers ( V O ⋅ ⋅ or Oi′′) and high mobility of these carriers.", "Since oxygen ion conduction takes place in the ABO3 perovskites by hopping through a triangle made up of two A-site and one B-site cations, the radii (rA, rB) and relaxations of these cations during oxygen migration impact the oxide ion mobility [37].", "Cherry et al. have noted that a tolerance factor, t = (rA + rO)/√2(rB + rO), of 0.81 corresponds to the minimum calculated oxygen migration energy, thought to be due to an optimum balance of relaxations between the A and B cations for this size ratio (i.e., smaller A-site cations and larger B-site cations) [38].", "Oxygen vacancy mobility may also be enhanced by more facile reduction of B site cations since transfer of some electron density from oxygen makes it smaller and more able to pass through the A-A-B cation triangle [39,40]; in this sense migration enthalpies may scale with oxygen vacancy formation enthalpies.", "Tensile strain has also been calculated to decrease the migration barrier for oxygen hopping in perovskites [41].", "The presence of cation vacancies and their induced disorder has additionally been suggested to increase the ionic mobility [42].", "On the other hand, one must also consider the possibility for trapping of carriers.", "Oxide ion mobility tends to be decreased when the oxygen defects (e.g., VO) are associated with other defects (e.g., acceptors) or otherwise ordered, e.g., by more non-uniform energy landscapes, such as created by cations with different sizes or electronegativities occupying a sublattice.", "Such effects add a dissociation enthalpy to the migration enthalpy in the conductivity exponential term, which may be overcome at high temperatures where the defects become dissociated or disordered.", "Larger binding energies of oxygen vacancies and acceptor dopants can contribute to larger overall conductivity activation energies at lower temperatures, and minimizing these binding energies (e.g., as for Sr La ′- V O ⋅ ⋅ pairs vs. other dopants in LaGaO3 and LaCoO3) requires optimizing both elastic strain and electrostatic effects of the dopant [37].", "Oxygen non-stoichiometry generally occurs as an ionic compensation mechanism to maintain charge neutrality upon introduction of charged point defects, such as aliovalent dopants, cation vacancies, anti-site defects, or change in valence state of multivalent cations.", "Many perovskite electrodes therefore intentionally contain acceptor dopants, such as Sr2+ on a La3+ site, having a relative negative charge, which can be ionically compensated by positively-charged oxygen vacancies: (3) M 2 O 3 + 2 SrO → LaMO 3 2 Sr La ′ + 2 M M × + 5 O O × + V O ⋅ ⋅ Such substitution can also be electronically compensated, in this case resulting in the formation of positively charged holes: (4) 1 2 O 2 + M 2 O 3 + 2 SrO → LaMO 3 2 Sr La ′ + 2 M M × + 6 O O × + 2 h ⋅ The presence of multivalent cations can support the electronic compensation mechanism and the electronic conductivity, though holes may not necessarily localize exclusively on the multivalent cation.", "Again, high mobility of the electronic carriers is also important for high electronic conductivity, and significant variety in the extent of charge localization on multivalent cations can be observed in perovskite electrodes.", "Increasing the concentration of multivalent cation is one way to increase the electronic mobility as the electronic states contributed by these ions broaden or overlap as the concentration increases.", "For example in the perovskite SrTi1−xFexO3−α, increasing the Fe content from x = 0.05 to 0.35 increases the hole mobility by about a factor of 10 [32,33,43].", "Similarly, in the perovskite La0.9Sr0.1Ga1−xNixO3−δ, the conductivity changes from predominantly ionic, to electronic hopping, to apparently metallic (electronic) upon increasing the Ni content to x = 0.5 [44].", "Aside from acceptor doping, smaller thermal band gaps can increase the intrinsic concentration of electronic carriers. 4.2.", "Bulk Chemistry Impact on Oxygen Surface Exchange In terms of oxygen surface exchange, the key to improving performance is to identify and improve the rate-limiting step, whether chemisorption/desorption, charge transfer, dissociation/association, or lattice incorporation/excorporation, since the slowest step dominates the reaction kinetics.", "Complicating factors include the issues that (1) these steps may occur somewhat simultaneously, such as in charge-transfer assisted adsorption or charge-transfer assisted dissociation; (2) many possible detailed reaction pathways exist; and (3) the rate-limiting step can change with operating conditions or over time, and is not always the same across different material systems.", "Therefore, creating comprehensive “design principles” or chemical descriptors for rapid oxygen surface exchange is not a simple process.", "Five approaches taken to tackle this challenge are given below with characteristic examples.", "Please note that these examples are intended as case studies of each approach but are not a comprehensive or exhaustive summary of work performed in this area. 4.2.1.", "Experimental Studies Seeking to Identify the Rate-Limiting Step for Particular Chemistries under a Limited Range of Conditions Merkle and Maier have demonstrated a method for homing in on the rate-determining step (RDS) for surface oxygen incorporation by combining spectroscopic information with both equilibrium and non-equilibrium measurements of oxygen exchange kinetics as a function of variables including oxygen partial pressure, temperature, and applied UV light intensity [45].", "Their method was applied to Fe-doped SrTiO3 single crystals, and the interpretations of the experimental results are enabled by a thorough understanding of the defect chemistry and electronic structure of this composition.", "Nonetheless, a similar experimental approach may be applied to other materials, bearing in mind that results and interpretations will necessarily be different in materials with different defect chemistry and electronic structures.", "The general approach is as follows: Intermediate adsorbed oxygen states such as the superoxide O2−, (more controversial) peroxide O22−, and O− radicals may be identified from techniques such as electron paramagnetic resonance (EPR), X-ray or Ultraviolet photoelectron spectroscopy (XPS/UPS), infrared (IR) spectroscopy, and electron energy loss spectroscopy (EELS), giving some insight into observable species present during the reaction.", "A selective dependence of the reaction kinetics on the intensity of UV light irradiation (with higher energy than the band gap) can indicate the role of electronic carriers in the RDS or a prior step (whether electrons or holes depends on which is the minority carrier that will be relatively more enhanced by exposure to UV light).", "The measured oxygen partial pressure (pO2)-dependence of the reaction rate for small pO2 steps (in equilibrium) and of the initial reaction rate for large pO2 steps (out of equilibrium) can be compared to what is predicted for each possible mechanism to provide information on the molecularity of oxygen (O2n− vs.", "On−) in the RDS and of the number of electrons transferred in or up to that point.", "For this SrTiO3:Fe system their results suggested the presence of O2n− in the RDS with one electron transferred; further, if the bulk and surface defect concentrations share the same pO2 dependence, those authors concluded that formation of O22− by electron transfer or dissociation of O22− is the most likely RDS under the measurement conditions.", "An important point from their work and that of others [46,47] is that the pO2 dependence of the reaction rate in equilibrium alone may not be sufficient to identify the fundamental, detailed RDS, since many mechanisms can share the same equilibrium pO2 dependence. 4.2.2.", "Experimental Studies Chemically Varying Point Defect Concentrations or Aspects of Electronic Structure to Identify Controlling Factors for the Surface Exchange Rate for a Particular Chemical System Tuller, Jung, Kim, Perry, and co-workers have also applied Sr(Ti,Fe)O3 as a model system for probing which aspects of bulk defect chemistry or the related electronic structure are key to fast oxygen surface exchange in this system [34,48,49,50,51].", "Isovalent or aliovalent substitution on the A- and B-sites of this perovskite results in changes in oxygen non-stoichiometry and electrical properties that can be measured and modeled to understand the changes in defect concentrations and Fermi level (from the electron and hole concentrations).", "Dense thin film electrodes deposited by pulsed laser deposition on electrolyte substrates have well-defined geometries enabling comparisons of electrochemically-measured surface exchange kinetics among different compositions (Figure 5).", "To date, work along these lines has demonstrated only very weak dependencies of kq (electrically or electrochemically driven surface exchange constant) on the ionic and (p-type) electronic conductivities, while the activation energy for kq scales with the position of the Fermi level relative to the conduction band (varied by changing the Fe content on the B site) [48].", "Since the minority electron concentration in the conduction band is exponentially dependent on the Fermi level position in this strongly p-type material, the result suggested that electron transfer from the electrode conduction band to the adsorbed oxygen was limiting the exchange kinetics.", "Subsequent work aimed at increasing the minority electron concentration through enhancing reducibility (via Ba substitution on the A-site) [32,50] and through donor doping (via La on the A-site) [34]; in both cases the apparent activation energy for kq was lowered.", "This result was attributed to the rise in bulk Fermi level, though bulk substitution may also change the surface catalytic activity by changing the cations in the outermost surface and sub-surface.", "Additionally, any expected small changes in absolute values of kq are difficult to measure owing to rapid “aging” of the electrodes [34,50], attributed to surface segregation (see also Section 4.4 and figure therein).", "Effects such as these will be discussed further in the section on surface chemistry.", "More recent work has aimed at modifying the mobility of the minority electrons in the conduction band, rather than their concentration, e.g., through substitution of Sn for Ti on the B-site [51].", "These controlled studies are important for identifying key defects and aspects of electronic structure; however, they do not indicate a detailed reaction mechanism.", "Additionally, Merkle and Maier have suggested that for this system, charge transfer is only limiting for low Fe contents [52], consistent with the caveat that key factors identified for a particular chemical system may not be broadly applicable; on the other hand, as for the approach in Section 4.2.1, this chemical substitution approach itself can be more broadly applied to various systems. 4.2.3.", "Compilations of Experimental Data, for a Variety of Electrode Materials, on Surface Exchange Coefficients as a Function of Materials Properties in Order to Find Correlations In an effort to identify more broadly which defect species or properties are predictors of, or limit, fast surface exchange, some reviews have compiled data from many electrode chemistries to identify correlations.", "Kilner may have been the first to point out a relationship between the tracer oxygen self-diffusion coefficient (D*) and tracer surface exchange coefficient (k*) both for fluorite-structured and perovskite-structured materials [53].", "Log(k*) showed, on average, a linear dependence on log(D*), though with different slopes for the two different structure types.", "Generally speaking, therefore, electrodes with higher oxygen self-diffusion may also exhibit higher surface exchange coefficients; however, there is considerable scatter in such plots.", "Wang et al. more recently published a similar plot of log(k*) vs. oxygen ion conductivity for various perovskites, showing again correlation but with wide scatter, particularly at lower ionic conductivity or k* values [54].", "Such studies broadly suggest the importance of oxygen vacancy availability for the surface exchange reaction (in oxygen sub-stoichiometric compounds), whether as a site for incorporation or as a donor enabling more facile charge transfer at the surface, assisting chemisorption and/or dissociation.", "Other early work by Boukamp et al. [55] noted the importance of electronic charge transfer in the surface exchange reaction broadly, comparing electronic conductivities and values of k for two fluorite compositions and mixed conducting perovskites in general.", "Though these data are limited, a plot of log(k*) vs. log(electronic conductivity) also suggests a linear relationship when plotted over a wide enough range.", "More recently, De Souza introduced an empirical expression for k* which indicated that high concentrations of electronic carriers (electrons and holes) and low concentrations of oxygen vacancies would lead to fast oxygen reactions at the surface, i.e., that donor-doped low band-gap materials or those with oxygen interstitial conduction would be better [56]. 4.2.4.", "Computational Studies of a Limited Range of Chemistries to Identify Key Aspects of Bulk Chemistry and Electronic Structure Vital for the Exchange Reaction Computational approaches have the advantage of being potentially a more rapid method to investigate structure-property relationships relating to surface reactions with atomistic insight and the disadvantage of being more challenging to apply to high temperature situations of potentially ambiguous surface chemistry.", "As an example of work in this area, density functional theory (DFT) calculations by Morgan’s group combined with electrochemical measurements in Shao-Horn’s group have suggested a correlation between the calculated bulk O 2p band center (vs. the Fermi level) of the electrode and its measured high temperature surface exchange kinetics (k* or kq), including the activation energy [57].", "Their work has so far encompassed several Ruddlesden-Popper and perovskite compositions.", "These groups suggested that this aspect of the bulk electronic structure could be a predictive descriptor for rapid surface exchange; on the other hand, a broad set of experimentally measured surface exchange data from the literature did not correlate clearly with the calculated bulk O 2p band centers, possibly due to variations in sample preparation or measurement approach.", "DFT simulations combined with nudged elastic band calculations have also provided more atomistic insight into the reaction pathway and energetics for oxygen incorporation for selected perovskite and Ruddlesden-Popper phases.", "Such work is described in detail in the later section on surface chemistry. 4.2.5.", "Computational Materials-by-Design Approaches to Identify with New Chemistries Predicted High Surface Exchange Rates on the Basis of Previously Identified Descriptors Once structure-property relationships, i.e., descriptors relating bulk chemistry to defect chemistry and electronic structure and ultimately to surface exchange kinetics, have been identified, the logical next step is to conduct computational searches for chemistries that exhibit this particular descriptor.", "Searches may make use of databases of both existing and predicted (but not synthesized) stable chemistries.", "Such studies can be accompanied by high-throughput experimental screening for suitable performance over a wide range of chemistries.", "Similar approaches have been applied recently to identify candidate perovskite chemistries for thermochemical water splitting [58] and metal alloy anode catalysts for low temperature fuel cells [59].", "D.", "Morgan’s group recently reported screening candidate SOFC cathode materials on the basis of the O 2p band center (for surface exchange kinetics), thermodynamic stability, and band gap (for electronic conductivity) [60]. 4.3.", "Bulk Chemistry Impact on Thermo-Chemo-Mechanical Stability A number of degradation mechanisms may take place within or around the oxygen electrode over time at elevated temperatures or during start-stop cycles, as described previously in Section 2 and Figure 2.", "One significant mechanism under investigation is the induction of stresses owing to chemical expansion, when electrode materials undergo changes in oxygen content (Δδ) causing local lattice dilation/contraction and chemical strain (εC) [16].", "For example, during the oxygen evolution reaction in sub-stoichiometric materials (reverse of Equation (1)), materials typically expand, as an oxygen vacancy is created and the compensating electronic charge concentration changes.", "Localization of electrons on multivalent cations (such as creating Ce3+ in place of Ce4+) drives the expansion.", "Failure modes including cracking and delamination can result [18], since the stresses generated can be significantly larger than the strength of the materials (particularly if flaws are already present) [17].", "Chemical stress mitigation may be achieved through altering operating/start-stop conditions, engineering component morphologies, or changing intrinsic materials properties including the strength, toughness, surface exchange coefficient, oxygen diffusivity, and coefficient of chemical expansion, CCE = εC/Δδ.", "Perry, Bishop, Marrocchelli and co-workers have been investigating which factors impact CCEs in the perovskite structure [16,35,43,61,62] which is currently the most widely-used structure in oxygen electrodes.", "Such factors may span many length scales, so a combination of atomistic simulations (density functional theory (DFT), molecular dynamics) with experiments at both the crystal structure (in situ X-ray diffraction, neutron diffraction) and macro-structure levels (thermogravimetric analysis, dilatometry) is applied.", "To date, some factors that have been identified as significantly impacting CCEs in perovskites include charge localization on cations [43,61], size of the oxygen vacancies [35], temperature [62], and crystal symmetry [61,63].", "Of these, charge delocalization may be the most promising approach, as it can be accomplished easily by increasing the concentration of the multivalent cation, which lowers the CCE [43,61] and simultaneously increases both the electronic conductivity and (at least sometimes) the surface exchange kinetics [33,44,49].", "On the other hand, such materials with higher concentrations of multivalent cation also typically exhibit larger changes in stoichiometry (Δδ) for a given pO2 or temperature change, which also contributes to the chemical strain [43,61].", "Figure 6 shows the impact of increasing the multivalent cation, to delocalize charge, on CCEs of two mixed conducting perovskite electrodes.", "The effective size of oxygen vacancies is also an important factor, since smaller oxygen vacancies lead to smaller CCEs upon oxygen loss by counteracting some of the cation expansion [64].", "A combination of first principles calculations, experimental data, and development of an empirical model recently led to some of the first determinations of the effective size of oxygen vacancies in perovskite oxides [35]; on average the vacancy tends to be about 97% the size of the oxide ion (cf. 72% in the fluorite structure [65]) but with considerable variation among different compositions.", "Learning how to tailor the oxygen vacancy size via bulk chemistry could enable better control of CCEs in this structure. 4.4.", "Relationship between Bulk and Surface Chemistry As described above, bulk chemistry is known to impact many oxygen electrode properties, including the oxygen surface exchange kinetics, but since this latter property takes place at the surface, the local chemistry in the outer atomic layers of the electrode should be considered.", "Surface chemistry can differ from bulk chemistry via effects including surface reconstructions, space charges, modified point defect formation energetics, polarity, segregation, and extrinsic adsorption and reactions forming new phases, but in each case, there is a relationship between the bulk and surface chemistries.", "(If bulk and surface chemistries were not somehow related, bulk chemical descriptors for fast surface exchange would not exist.)", "Both experimental and computational approaches are providing insight into this relationship.", "For example, recent computational work by Lee and Morgan has demonstrated how different transition metal cations’ redox activity and surface polarity of different compositions lead to very different surface defect chemistry and surface properties of perovskites [66].", "Another example relating bulk and surface chemistry is the case where elastic and electrostatic effects within the bulk of the electrodes can contribute to the driving force for intrinsic surface segregation, where excess A-site cations enter the surface region as enrichment or secondary phases.", "Lee et al.", "(different authors) demonstrated the important roles of both elastic and electrostatic effects in A = (Sr, Ca, Ba) segregation in acceptor-doped (La, A2+)MnO3 both computationally using DFT and experimentally using analysis of thin film electrode surface morphology, chemistry, and electronic structure after high temperature anneals [67].", "In this composition, as with many oxygen electrodes, some A-site cations are acceptor dopants exhibiting a relative negative charge within the lattice, so they can be electrostatically attracted to positively-charged oxygen vacancies in the surface region.", "Additionally, the results demonstrated the clear influence of elastic effects, as segregation was more severe the larger (more size-mismatched vs.", "La) the acceptor cation was, i.e., in the order Ba > Sr > Ca, and segregation was less severe when the lattice expanded in lower oxygen partial pressures, better accommodating the larger dopants.", "More recently, preliminary studies by Perry indicate that electrochemically measured deterioration of surface exchange coefficients (kq)—see Figure 7—occurs more rapidly for larger A-site cations even when the cation is not an acceptor dopant (i.e., isovalent substitution) within thin film (Sr,A)Ti0.65Fe0.35O3−δ, A = Ba, Sr, Ca.", "In this latter case, different mechanisms of aging among these various cations on the surface could also influence the results, in addition to the degree of segregation.", "Nonetheless, results such as these suggest that smaller A-site cations may thermodynamically limit segregation or deterioration of surface exchange kinetics, even though from a kinetic perspective they should be able to diffuse to the surface faster.", "A-site cation deficiency has also been used as a method both of intrinsic acceptor doping and surface segregation prevention [68].", "However when some intrinsic or extrinsic surface poisoning is unavoidable, introduction of “gettering” species within the electrode composition is a promising alternative method to counter the negative effects of surface chemical changes on surface redox kinetics.", "Recent work by Zhao et al. demonstrated this approach, where La was introduced both on the surface and in the bulk of a (Ce,Pr)O2−δ electrode to react with Si poisoning on the surface and restore fast oxygen exchange kinetics; a further catalytic effect of La cannot be ruled out, however [69].", "Further details concerning characterization of surface chemistry in general are given in the section below. 5.", "Role of Surface Chemistry Surface chemistry is expected to play a critical role in the oxygen surface exchange process, yet relatively more attention has in the past focused on bulk electrode chemistry, with the implicit assumption that the surface is a simple termination of the bulk, containing transition metal cations for catalytic activity.", "However, recent focused studies of electrode surface chemistry, taking advantage of advances in surface characterization techniques, have enabled identification of significant differences in surface and near-surface compositions vs. the bulk, particularly after or during exposure of electrode materials to typical operation temperatures [70,71,72,73].", "A number of techniques have been developed to probe, in situ or in operando, the bulk and surface chemistry of oxygen electrodes during exposure to realistic operating temperature, gas atmosphere, and/or polarization conditions.", "Techniques include those based on X-ray diffraction [74,75,76], X-ray fluorescence [77], X-ray absorption spectroscopy [78], neutron diffraction [79] (largely for bulk information), “ambient pressure” X-ray photoelectron spectroscopy [80] and photoelectron microscopy [81], Raman spectroscopy [82], scanning probe microscopy [83], and environmental scanning or transmission electron microscopy [84].", "Each of these methods may be coupled with simultaneous ac-impedance spectroscopy measurement of half or full cells to correlate the electrochemical performance and degradation of the electrodes with the changes in local chemistry and structure [79].", "A comprehensive review of results from all of these techniques is beyond the scope of the present paper, and the interested reader is directed to the references mentioned herein for further information.", "Among recent developments in surface analysis and ion scattering methods, ion beam-based techniques including low energy ion scattering (LEIS) and time-of-flight secondary ion mass spectrometry (SIMS) techniques have proved to be particularly useful probes of the surface composition.", "Beneficial features of ion beam-based techniques include: (1) shallow (surface-sensitive) information depths because ions in the relevant energy ranges do not penetrate into a solid as far as X-ray or electron beams and (2) mass-sensitivity, thus enabling identification of isotopes as well as elements.", "Indeed, SIMS analysis of 18O isotopic tracer diffusion profiles in samples having undergone anneals in gaseous 18O at high temperatures has been used for several decades to derive the tracer oxygen exchange coefficient (k*) and diffusivity (D*) in ionic and mixed conductors [85,86].", "I2CNER in Kyushu University provides a unique environment for ion beam surface analysis.", "In this section, examples of results of surface analysis of oxygen electrodes will be briefly introduced, mainly focusing on (La,Sr)(Co,Fe)O3 perovskite oxide.", "As mentioned earlier, the composition La0.6Sr0.4Co0.2Fe0.8O3−δ (LSCF), which shows good ionic and electronic conductivities [87], along with high diffusivity and surface exchange coefficients, is a popularly used oxygen electrode of intermediate temperature SOFCs [88].", "This material is adopted as a model system to demonstrate ways in which LEIS and SIMS techniques can assist investigations of the relationship between surface chemistry and oxygen surface exchange kinetics. 5.1.", "Application of 18O Diffusion Profile Measurements by SIMS One question in the study of electrode surfaces is the extent to which crystal orientation or surface termination influences the surface exchange kinetics and diffusivity in the electrode, determining its performance.", "This question has been addressed for the highly anisotropic Ruddlesden-Popper structured electrodes by SIMS analysis of 18O profiles in epitaxial thin films grown with different orientations.", "For example, by this approach (La,Sr)2CoO4 was demonstrated by Chen et al. to exhibit faster oxygen diffusion along the ab-plane than the c-axis, but the surface exchange kinetics of films grown in the (001) and (100) orientations were not significantly different.", "The result was attributed to Sr segregation on both terminations, slowing oxygen incorporation [89].", "Another approach to study this question is to take advantage of finer focusing of the SIMS incident ion beam (e.g., Ga ion gun in FIB-SIMS) to enable depth profiling within individual grains presumably exhibiting different orientations in polycrystalline ceramic samples (it should be noted that a conventional SIMS primary ion beam analyzes areas on the order of hundreds of microns, much larger than the size of typical ceramic grains or electrode particles).", "One limitation with this approach is that the depth that can be measured is limited to approximately the lateral dimensions of the sputtered crater, owing to loss of signal for deeper craters.", "An example of this method applied to a dense LSCF ceramic, with 18O exchange at 723 K, is shown in Figure 8, after [90] by Druce et al.", "While not nearly as anisotropic as the aforementioned layered structures, the perovskite LSCF exhibits slight rhombohedral distortions, and different surface terminations of different grains, having different sites and energetics for oxygen adsorption, dissociation, and incorporation may be possible.", "Further details of the analysis and fitting are given in [90].", "Fits to the depth profiles within the grains and a macroscopic profile are shown as solid lines in Figure 8b, and the D* and k* values extracted from these fits (from [90]) are summarized in Figure 9.", "While the k* values within individual grains are slightly higher than the macroscopic k* value, they and the D* values do not vary much from grain to grain.", "Again, similar surface chemistry as a result of Sr segregation may be a factor in this result, as discussed in the later section on LEIS.", "While the results in Figure 8 and Figure 9 were obtained using a relatively high energy Ga ion beam, better depth resolution in addition to the already higher lateral resolution, may be obtained in some materials systems using Cs+ or C60+ sputtering [91,92].", "Another question relating to electrode surface chemistry and performance is the extent to which strain state may be tuned to optimize surface exchange kinetics.", "Again epitaxial thin film model electrodes, such as deposited by PLD, are an asset in performing fundamental studies, as strain can be induced by the energetic growth process and/or by coherent lattice mismatch with the substrate or adjacent layers (accounting for thermal and chemical expansion).", "Beyond enhancements in oxide ion mobility [41] or incorporation kinetics that may be derived by stretching the lattice through which the ion passes, there is also a chemo-mechanical coupling in many systems, whereby the applied strain can lead to changes in point defect chemistry [93].", "Both of these effects could, in principle, alter surface oxygen incorporation/excorporation energetics.", "Again, tracer 18O isotope diffusion profiles, measured ex situ by SIMS, as well as electrochemical impedance measurements, are providing some insight into the magnitude of the effect.", "For example in-plane tensile strain has been shown to accelerate both k* and D* into (100)-oriented epitaxial La1−xSrxCoO3−δ [94] and to improve kq, increase the oxygen interstitial concentration, and stabilize the surface chemistry in the anisotropic Nd2NiO4+δ Ruddlesden-Popper phase with tensile strain along the c-axis [95].", "Multilayer electrode structures are also the subject of research into strain effects; for example, Hyodo et al. fabricated a “laminated film” with layers of Cu and Ga-doped Pr2NiO4 (PNCG) and Sm-doped CeO2 (SDC), where the former phase was expected to be in compression and the latter in tension on the basis of lattice parameters [96].", "Using 18O tracer diffusion, the results suggested that mechanical strain has a large influence on the oxygen diffusivity; however, the enrichment in surface 18O concentration was more significant.", "Therefore, surface activity seemed to be more sensitively affected by mechanical strain effects in that system. 5.2.", "Evaluation of Surface Chemistry by LEIS LEIS measurements are able to identify elements in the outermost atomic monolayer, and this extreme surface sensitivity is of interest for understanding the composition immediately in contact with gaseous oxygen during the exchange process.", "Like SIMS, LEIS is often performed ex situ, where it can be applied to study electrode materials after treatment in high temperatures and gas atmospheres typical of operation conditions [70,97,98,99,100].", "While one expects qualitative similarities in the ex situ results on polycrystalline, dense ceramics or thin films and the surface chemistry of real, porous ceramic electrodes in operando, some differences owing to the microstructure and environment changes (e.g., surface-to-volume ratio, surface curvature, grain boundary density, impurity gas concentration, impact of adjacent cell layers, etc.) may be possible.", "In this regard, an additional advantage of LEIS is that there are few limitations in the form of the sample; real porous electrodes may be studied as well as model systems such as dense ceramics or thin films.", "One outcome of the model sample, ex situ studies has been the confirmation of A-site cation termination/segregation widely observed in the SOFC/SOEC/catalysis community using a variety of other approaches that have slightly less surface sensitivity, such as total reflection X-ray fluorescence, nanoprobe Auger spectroscopy, SIMS, scanning electron microscopy with energy-dispersive spectroscopy, and X-ray photoelectron spectroscopy [73,101,102,103,104].", "For example, Figure 10, taken from [97], shows a series of LEIS spectra of LSCF ceramic samples; one has been measured after polishing, and the others were measured after annealing for 8 h at different temperatures.", "In Figure 10a, the peaks in the spectrum for the as-polished sample correspond to all the elements present in the bulk composition—O (1181 eV), Fe (2311 eV) and Co (2342 eV; these cannot be resolved with the He beam due to similar masses), Sr (2541 eV), and La (2701 eV).", "(Peak energies quoted correspond to the high energy onset of the peaks, and the peak apexes appear at slightly lower energies due to inelastic scattering processes.)", "Peak intensities for surface elements are proportional to their coverage (by a sensitivity factor dependent on the element’s mass), and so changes in their intensities are indicative of changes in outermost surface coverage.", "From the other spectra in Figure 10a, it can be seen that with progressively higher annealing temperatures, the coverage of Sr increases at the expense of those of La and the transition metal cations.", "In Figure 10b, quantified peak areas from Figure 10a are plotted to show the evolution of surface coverage in terms of cation ratios for given annealing temperatures.", "The increase of Sr coverage is most pronounced between 673 and 873 K under these conditions; this result helps to explain the relative insensitivity of k* to LSCF grain orientation discussed earlier, since that sample was at 723 K for the 18O exchange.", "A sequence of LEIS spectra can also be obtained after stepwise removal of material by low energy (500 eV) Ar ion sputtering to provide depth profiles of elements.", "By this approach, one may, for example, study not only the outer monolayer chemistry but also the sub-surface region after Sr surface enrichment/segregation has occurred.", "Figure 11 (from [98]) shows sample LEIS spectra (partial energy range) at different depths and a resulting depth profile measured on a LSCF ceramic sample after annealing for 12 h at 1273 K.", "While the outermost surface is characterized by an absence of La or transition metal cations in Figure 11a (though there is evidence for sub-surface La indicated by the rise in background signal below 3500 eV), the La, Co, and Fe peaks appear in the outer monolayer analyzed after removal of some material.", "The depth profile in Figure 11b demonstrates not only the B-site deficient surface region but also a sub-surface region slightly enriched in the B-site cations.", "This enrichment was shown to be more pronounced in GdBaCo2O5+δ (GBCO) and La2NiO4+δ (LNO) [98], which also lacked transition metal cations in the initial outer monolayer.", "Interestingly, various oxide structures (perovskite, double perovskite, Ruddlesden-Popper, fluorite) and chemistries exhibit surfaces enriched with rare earth or alkaline earth cations with larger ionic size and smaller oxidation number than their hosts.", "As discussed earlier in the section discussing the relationship between bulk and surface chemistry, this surface enrichment phenomenon may in principle be explained by a combination of elastic and electrostatic effects with possible influence from extrinsic factors, such as gas atmosphere.", "It should also be noted that while these particular LEIS measurements have been performed on ceramic pellets after heat treatments, they may also be carried out on electrochemical cells after testing, to provide some insight into the impact of surface chemistry on actual electrode performance, particularly oxygen surface exchange rate.", "Finally, surface chemistry studies by other methods have also indicated that the intrinsic segregation phenomena may interact with extrinsic poisoning effects to alter surface chemistry.", "A common impurity in the gas stream for the SOFC cathode is S.", "Although the aforementioned LSCF composition is now popularly used as the oxygen electrode of SOFCs and SOECs, this oxide is sensitive to the presence of the S impurity, with which it reacts, resulting in the electrode surface deactivation.", "Figure 12 shows scanning electron microscopy (SEM) images of LSCF electrodes having been exposed to impurity sulfur during power generation and degradation measurements [105].", "Evidently, regions appearing to have partially melted, where high amounts of S and Sr are detected, are observed (these are the darker spots in Figure 12a).", "Therefore, it appears that surface segregated Sr may easily react with SO2 in the air to form SrSO4 which easily sinters and blocks the surface from participating in efficient oxygen reduction.", "Therefore, one reason for degradation of oxygen electrodes is caused by a combination of intrinsic surface segregation of Sr and extrinsic S poisoning, and this process appears relatively acute for LSCF. 5.3.", "Modeling of Oxygen Dissociation on Surfaces Absent of Transition Metal Cations In light of the emerging experimental evidence among the ionics community of A-site segregation and AO termination in perovskites and related structures under typical SOFC/SOEC operating conditions, computational simulations have been applied to understand the mechanism of oxygen exchange on surfaces absent of transition metal cations.", "Density functional theory calculations can estimate the energy of various configurations of an electrode slab interacting with oxygen, to determine, for example, the lowest energy oxygen adsorption site(s), whether those configurations indicate associated or dissociated oxygen, and whether such a process is energetically spontaneous.", "In addition, transition state analysis by nudged elastic band calculations can indicate the activation energy barriers for moving between one step in the reaction to the next.", "These approaches have recently been applied to study oxygen chemisorption and dissociation on SrO-terminated SrTiO3 and LaO-terminated La2NiO4, both for the stoichiometric and oxygen-deficient compounds, where oxygen vacancies are introduced via ionically compensated acceptor doping with Fe in the case of SrTiO3.", "Details of the calculation approaches are given elsewhere [106,107].", "Both oxygen chemisorption and dissociation may be enabled by charge transfer to the oxygen, so the presence of accessible electron density in or near the surface can help these processes to occur.", "In both SrO-terminated SrTiO3 and LaO-terminated La2NiO4, the presence of oxygen vacancies near the surface was shown to facilitate (lower the energy barrier for) oxygen adsorption and dissociation on the surfaces, by enabling charge transfer.", "In the case of SrO terminated stoichiometric SrTiO3, oxygen chemisorption and dissociation was not energetically favorable, since the closed-shell configuration of Sr2+ does not contribute electron density that would interact with chemisorbed oxygen.", "For LaO-terminated stoichiometric La2NiO4, however, oxygen chemisorption was shown to be exothermic (−0.73 eV and −0.59 eV for chemisorption on a slip position and La-La bridge position, respectively), because the extra 5d electron in La3+ can polarize its 6s valence orbitals and enable charge transfer from the surface, destabilizing the oxygen molecule.", "Calculated energetics for dissociation of oxygen after chemisorption on the aforementioned surfaces are summarized in Table 1. 6.", "Conclusions 6.1.", "Summary Oxygen electrodes, typically mixed conducting perovskites and related structures, play a vital role in impacting the efficiency and lifetime of SOFCs/SOECs as the location of electrochemical oxygen incorporation or evolution.", "They need to demonstrate excellent catalytic activity for rapid surface oxygen exchange, good bulk transport properties (electronic and ionic), and maintain thermo-chemo-mechanical stability in contact with other cell components and often impure gas atmospheres for multiple years of operation including start-stop cycling.", "In this non-exhaustive review we have highlighted some of the work at I2CNER, Kyushu University, set in the context of work in the broader community, which seeks to understand the roles of bulk and surface chemistry in these aspects of oxygen electrode performance.", "Understanding the impact of bulk composition on carrier concentrations and mobilities, surface exchange kinetics, and chemical expansion coefficients remains an active area of research, both experimentally and computationally.", "At the same time, an understanding of the relationship between bulk and surface chemistry is being developed through computational simulations and experimental high resolution and/or operando surface chemistry studies, that may assist design of electrodes with more robust surface chemistries that are impurity tolerant or do not show rapid surface segregation.", "As cross-cutting approaches, the use of strain and/or a high density of active interfaces show promise for enhancing bulk transport and surface exchange kinetics. 6.2.", "Outlook Although fuel cells using solid ceramic electrolytes have been in development for over 60 years, there remain significant opportunities for improving the efficiency and durability of oxygen electrodes in these SOFCs and in the newer SOEC technologies.", "Concerning bulk chemistry, the area of “electro-chemo-mechanics”, i.e., the coupling between mechanical, chemical, and electrical states of materials, is an emerging research theme underlying electrode performance improvements, including (1) enhancements in transport and surface reactivity realized by tailoring strain state (mechano-electrical and mechano-electrochemical coupling) as well as (2) mitigation of deleterious chemical expansion during operation, induced by stoichiometry changes (chemo-mechanical coupling).", "In the case of intentionally applied strain (1), an understanding of how to realize high levels of durable strain in the appropriate direction(s) in real electrodes under operating conditions should be pursued, and an understanding of what magnitude of enhancements in oxide ion mobility, non-stoichiometry, and surface exchange kinetics can be accomplished realistically in devices, given the modest strain levels that can be realized in brittle ceramics, should be developed.", "At a fundamental level, partial understanding of oxygen mobility in perovskites has been developed, but further insight into how cation polarizability, ionic radii, tolerance factor, free volume, lattice strain, interfacial effects, and other factors can be optimized for the fastest possible ionic mobility should be developed in the future.", "Concerning chemical expansion (2), further insight into factors impacting the magnitude of coefficients of chemical expansion is needed, and modeling of chemical stress development spanning atomic to device length scales would help to mitigate these stresses and maximize device mechanical integrity for high durability.", "Regarding surface chemistry and oxygen surface exchange kinetics, areas of particular interest are: (1) clarifying rate-limiting steps and mechanisms of oxygen incorporation/excorporation with atomistic insight both experimentally and computationally; (2) exploiting the unique properties of hetero-interfaces, grain boundaries, and other long range defects intersecting the surface; (3) identifying the theoretical optimal composition(s) for the outermost atomic monolayers; and (4) learning how to control the outermost chemistry in operating conditions via bulk and surface chemical tailoring.", "Each of those areas is particularly strategic because the high activation energy of the oxygen exchange process limits the operating temperature range of the devices at present and can dominate efficiency losses at lower temperatures.", "For practical use of SOFCs/SOECs, an additionally important challenge is increasing the long-term stability.", "Therefore many research efforts are aimed at identifying, understanding, and addressing degradation mechanisms that lead to increases in internal resistances and overpotentials during operation.", "For example, learning how to control and mitigate electrode surface poisoning, either by intrinsic large cation segregation or by extrinsic species depositing or reacting with the surface is a particularly significant area of research along these lines.", "Overall, oxygen electrode development remains a very active field, and continued effort to understand fundamental structure-property relationships in both the bulk and surface of electrodes is needed for development of descriptors for rational design and discovery of superior electrode chemistries." ]

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[ "Novel Mg-Doped SrMoO3 Perovskites Designed as Anode Materials for Solid Oxide Fuel Cells Novel Mg-Doped SrMoO3 Perovskites Designed as Anode Materials for Solid Oxide Fuel Cells CascosVanessa1*AlonsoJosé Antonio1Fernández-DíazMaría Teresa2 MenzlerNorbert H.", "Academic Editor 1Instituto de Ciencia de Materiales de Madrid, CSIC, Cantoblanco, 28049 Madrid, Spain; jaalonso@icmm.csic.es 2Institut Laue Langevin, BP 156X, Grenoble 38042, France; ferndiaz@ill.fr *Correspondence: vcascos@icmm.csic.es; Tel.: +34-91-334-9000; Fax: +34-91-372-0623 588 SrMo1−xMxO3−δ (M = Fe and Cr, x = 0.1 and 0.2) oxides have been recently described as excellent anode materials for solid oxide fuel cells at intermediate temperatures (IT-SOFC) with LSGM as the electrolyte.", "In this work, we have improved their properties by doping with aliovalent Mg ions at the B-site of the parent SrMoO3 perovskite.", "SrMo1−xMgxO3−δ (x = 0.1, 0.2) oxides have been prepared, characterized and tested as anode materials in single solid-oxide fuel cells, yielding output powers near 900 mW/cm−2 at 850 °C using pure H2 as fuel.", "We have studied its crystal structure with an “in situ” neutron power diffraction (NPD) experiment at temperatures as high as 800 °C, emulating the working conditions of an SOFC.", "Adequately high oxygen deficiencies, observed by NPD, together with elevated disk-shaped anisotropic displacement factors suggest a high ionic conductivity at the working temperatures.", "Furthermore, thermal expansion measurements, chemical compatibility with the LSGM electrolyte, electronic conductivity and reversibility upon cycling in oxidizing-reducing atmospheres have been carried out to find out the correlation between the excellent performance as an anode and the structural features. anode IT-SOFC SrMoO3 perovskite neutron diffraction 1.", "Introduction Solid oxide fuel cells at intermediate temperatures (IT-SOFC) are electrochemical devices able to convert the energy involved in the combustion of a fuel directly into electrical energy.", "IT-SOFCs work at intermediate temperatures, typically between 700 °C and 850 °C; therefore, the reaction kinetics is extremely favored, and the efficiency of the energy conversion process is very high, compared to other low-temperature fuel cells.", "The fuel oxidation reaction in SOFC happens in the anode.", "SOFCs often use anodes based on Ni-YSZ (yttria-stabilized zirconia) and Ni-LDC (lanthanum-dope ceria) cermets.", "These composite anodes have an excellent catalytic activity for the fuel-oxidation reaction and high electronic and ionic conductivity, but unfortunately, these materials promote carbon formation during the direct oxidation of hydrocarbon fuels and suffer from sintering problems during the cell operation [1,2,3].", "Furthermore, Ni-based anodes have the disadvantage of being contaminated with H2S traces contained in H2 [4].", "In order to avoid the problems associated with the cermet-based anodes, single-phase active materials have been investigated with the ABO3 perovskite structure.", "By suitably choosing stable oxide compounds in reducing atmospheres, these materials can provide enough electronic and ionic conductivity to perform as anodes in IT-SOFC.", "The SrMoO3 cubic perovskite with Mo4+ at the octahedral B positions has an extremely high electrical conductivity at room temperature (104 S∙cm−1 [5]); moreover, molybdenum is a very suitable element to catalyze the fuel-oxidation reaction.", "Unfortunately, this oxygen-stoichiometric oxide cannot exhibit the required oxygen-ion diffusion and conductivity.", "In previous works, the Mo ions were partially replaced by 10% and 20% aliovalent elements, namely Fe3+ and Cr3+ [6,7], thus inducing the creation of oxygen vacancies in the perovskite material.", "We demonstrated that Fe and Cr doping promotes the ionic conductivity of these oxides, thus combining excellent mixed ionic and electronic conduction (MIEC) properties that make them excellent anode materials.", "Following the same strategy, taking advantage of the excellent metallic conduction properties of SrMoO3, in the present work, we show that doping with aliovalent Mg2+ ions at the B-site is also extremely effective for the mentioned purpose.", "Mg2+ ions were chosen because they are able to adopt an octahedral coordination in a perovskite structure, and the large ionic size (0.72 Å) [8] may lead to an expansion of the unit-cell dimensions, thus promoting the ionic diffusion across the solid.", "Additionally, avoiding the use of transition metals (like Fe3+ and Cr3+) in the anode could prevent the diffusion across the electrolyte and hinder the induction of electronic conductivity.", "Moreover, the use of Mg2+ is perfectly compatible with the electrolyte LSGM, also containing this element.", "In the present case, 10% and 20% Mg2+ were introduced in the perovskite, developing new mixed conductors with potential application as anodes in SOFCs at intermediate temperature.", "SrMo1−xMgxO3−δ (x = 0.1 and 0.2) materials have been prepared and characterized by different techniques, and finally, their performance was evaluated as anodes in a test cell, using SrCo0.8Fe0.2O3−δ (SCFO) as the cathode and LSGM as the electrolyte.", "The structural characterization was carried out from an in situ temperature-dependent neutron powder diffraction (NPD) study in the 25–800 °C range, under the actual working conditions of a SOFC.", "Additionally, thermal expansion, chemical compatibility, electrical conductivity and the reversibility of the oxidation-reduction process were also investigated. 2.", "Experimental Section SrMo1−xMgxO3−δ (x = 0.1, 0.2) polycrystalline samples were synthesized by soft-chemistry procedures.", "Stoichiometric amounts of Sr(NO3)2, (NH4)6Mo7O24·4H2O and Mg(NO3)2·6H2O were dissolved in a 10% citric acid solution (50 g of citric acid dissolved in 500 mL of water).", "After removing the solvent by gentle heating, the formed organic resins were decomposed at 600 °C for 12 h in air.", "Oxidized scheelite phases of composition SrMo1−xMgxO4−δ, containing Mo6+ ions, were identified by XRD after the treatment at 600 °C in air.", "A final treatment at 1050 °C in a tubular furnace under a H2 (5%)/N2 flow for 15 h led to the formation of the reduced perovskite oxide.", "The initial characterization of the product was carried out by X-ray diffraction (XRD) with a Bruker D8 Advanced diffractometer (40 kV, 30 mA), controlled by DIFFRACTPLUS software, in Bragg–Brentano configuration with CuKα radiation (λ = 1.5418 Å ) and a PSD (position-sensitive detector).", "A filter of nickel allows the complete removal of CuKβ radiation.", "The data were obtained between 10° and 64° in steps of 0.02°.", "NPD data were collected in the diffractometer D2B at the Institut Laue-Langevin, (Grenoble, France), with a neutron wavelength λ = 1.594 Å within the angular 2θ range from 10°–160° for x = 0.1, and at the HRPT diffractometer of the SINQ spallation source (PSI, Villigen, Switzerland), with λ = 1.494 Å within the 2θ range from 10°–164° for x = 0.2.", "About 2 g of the samples were contained in vanadium cans and studied at 25 °C.", "For the temperature-dependent study, a selected sample contained in a vanadium cylinder was placed in the isothermal zone of a furnace with a vanadium resistor operating under vacuum (PO2 ≈ 10−6 Torr) coupled to the D2B diffractometer.", "The measurements were carried out at 25, 200, 400, 600 and 800 °C for x = 0.1.", "In all cases, the collection times were 2 h per pattern.", "The diffraction data were analyzed by the Rietveld method [9] with the FULLPROF program [10] and the use of its internal tables for scattering lengths.", "The line shape of the diffraction peaks was generated by a pseudo-Voigt function.", "In the final run, the following parameters were refined: scale factor, background coefficients, zero-point error, pseudo-Voigt corrected for asymmetry parameters and positional coordinates.", "Isotropic thermal factors for all of the metal atoms and the anisotropic ones for oxygen atoms were also refined for the NPD data.", "The coherent scattering lengths for Sr, Mo, Mg and O were 7.02, 6.715, 5.375 and 5.805 fm, respectively.", "Thermal analysis was carried out in a Mettler TA3000 system equipped with a TC15 processor unit.", "Thermogravimetric (TG) curves were obtained in a TG50 unit, working at a heating rate of 10 °C∙min−1, in an O2 flow of 100 mL·min−1 from 35–900 °C using about 50 mg of sample in each experiment.", "Measurements of the thermal expansion coefficient and electrical conductivity required the use of sintered samples.", "For this purpose, pellets of SrMo1−xMgxO3−δ (x = 0.1, 0.2) were prepared by pressing the powder in dies and sintering in air at 950 °C for 12 h; finally, the pellet was placed in a tube furnace with 5% H2/95% N2 flow for 15 h at 900 °C.", "The densities of the pellets were around 70%–75% of the crystallographic value, calculated from the mass and geometrical volume.", "Thermal expansion of the sintered samples was carried out in a dilatometer Linseis L75/H, between 100 and 900 °C in H2(5%)/N2(95%).", "The conductivity was measured between 25 and 850 °C in H2(5%)/N2(95%), by the four-point method in bar-shaped pellets under DC currents of 100 mA.", "The currents were applied and collected with a Potenciostat-Galvanostat AUTOLAB PGSTAT 302, ECO CHEMIE.", "Single-cell tests were made on electrolyte-supported cells with La0.8Sr0.2Ga0.83Mg0.17O3−δ (LSGM) as the electrolyte, SrCo0.8Fe0.2O3−δ (SCFO) as the cathode material and SrMo1−xMgxO3−δ (SMMO) as anode material.", "The LSGM pellets of 20 mm in diameter were sintered at 1450 °C for 20 h and then polished with a diamond wheel to a thickness of 300 μm.", "La0.4Ce0.6O2−δ (LDC) was used as a buffer layer between the anode and the electrolyte in order to prevent the interdiffusion of ionic species between perovskite and electrolyte.", "Inks of LDC, SMMO and SCFO were prepared with a binder (V-006 from Heraeus, Hanau, Germany).", "LDC ink was screen-printed onto one side of the LSGM disk followed by a thermal treatment at 1300 °C in air for 1 h.", "SMMO was subsequently screen printed onto the LDC layer and fired at 1100 °C in air for 1 h.", "SCFO was finally screen printed onto the other side of the disk and fired at 1050 °C in air for 1 h.", "The thickness of the anode and cathode was 10 μm.", "The working electrode area of the cell for both the anode and cathode was 0.25 cm2 (0.5 cm × 0.5 cm).", "Pt gauze with a small amount of Pt paste in separate dots was used as the current collector at both the anodic and the cathodic sides for ensuring electrical contact.", "The cells were tested in a vertical tubular furnace at 800 and 850 °C; the anode side was fed with pure H2, with a flow of 20 mL·min−1, whereas the cathode worked in air.", "The fuel-cell tests were performed with an AUTOLAB 302N Potentiostat/Galvanostat by changing the voltage of the cell from 1.2–0.1 V, with steps of 0.010 V, holding 10 s at each step.", "Current density was calculated by the recorded current flux through the effective area of the cell (0.25 cm2).", "Each VI (voltage-intensity) scan corresponds to one cycle; the activation of the cell was followed in subsequent cycles until the full power of the single cell was reached. 3.", "Result and Discussion 3.1.", "Crystallographic Characterization The initial characterization of the products was carried out by XRD.", "SrMo1−xMgxO3−δ (x = 0.1, 0.2) compounds were obtained as well-crystallized powders.", "The SrMoO3 phase was also prepared as a reference.", "Figure 1 shows the XRD patterns of the SrMo1−xMgxO3−δ (x = 0, 0.1 and 0.2) oxides.", "The XRD diagrams are characteristic of a cubic perovskite structure with the Pm-3m group.", "The unit-cell parameters obtained for x = 0, 0.1 and 0.2 are 3.9760(3), 3.9739(4) and 3.9654(2) Å, respectively.", "No impurity phases were detected in any samples.", "In order to perform a more comprehensive structural study for the SrMo1−xMgxO3−δ (x = 0.1 and 0.2) series, an investigation by NPD at room temperature (RT) for the SrMo1−xMgxO3−δ family and high temperature (up to 800 °C) for SrMo0.9Mg0.1O3−δ was carried out.", "The structures were refined in the Pm-3m group (No. 221), with Z = 1.", "Sr atoms are located at the 1b (1⁄2, 1⁄2, 1⁄2) position; Mo and Mg atoms are randomly distributed at 1a (0, 0, 0) sites; and the O oxygen atoms are placed at the 3d (1⁄2, 0, 0) position.", "A small oxygen deficiency was observed at room temperature after refining the occupancy factors of the oxygen atoms.", "After the complete refinement of the SrMo1−xMgxO3−δ (x = 0.1 and 0.2) crystal structures, a good agreement between the observed and calculated NPD patterns at room temperature is shown in Figure 2.", "Table 1 lists the unit-cell, atomic positions, occupancies, displacement parameters, discrepancy factors and interatomic distances after the Rietveld refinements of doped samples at room temperature.", "The unit-cell parameters decrease as the amount of Mg in the sample increases.", "The (Mo,Mg)-O1 bond lengths at room temperature decrease accordingly with Mg-doping from 1.98814(1) Å for the undoped sample to 1.98247(3) Å for the sample with x = 0.2.", "This happens even though the ionic size of Mg2+ (0.72 Å) is higher than Mo4+ (0.65 Å) [8].", "This fact may suggest that a unit-cell contraction is happening because oxygen vacancies are being created when Mo is partially replaced by Mg, but it is more probable that this cell contraction is related to a partial oxidation of Mo ions (hole doping effect) as Mg2+ is introduced into the perovskite, resulting in a mixed-valence state Mo4+-Mo5+ proportional to the doping rate.", "There are well-known Mo-containing double perovskites (e.g., Sr2FeMoO6) reported to have Mo5+ions, exhibiting Mo5+-Mo6+ mixed valence [12].", "Similar unit-cell contraction was observed in previous studies of SrMoO3 doped with 10%, 20% and 30% Fe, where the ionic size of high-spin Fe3+ is practically the same as Mo4+, and the cell is considerably shrunken [6] at room temperature.", "On the other hand, the oxygen occupancy also evolves with Mg2+ doping, being slightly deficient for x = 0.1 (2.985(3) O per formula unit) and significantly more deficient for x = 0.2 (2.856(3) per formula unit) at room temperature.", "The thermal evolution of the crystal structure under the anode conditions of an SOFC was studied by NPD for the x = 0.1 oxide.", "The NPD patterns are illustrated in Figure 3.", "No structural transitions in the temperature range under study (25–800 °C) were found.", "Figure 4 illustrates the good agreement between the observed and calculated NPD patterns for the sample with x = 0.1 at 400 and 800 °C.", "Table 2 includes the structural parameters after the refinement of the SrMo0.9Mg0.1O3−δ structure at the different temperatures under study.", "Figure 5a shows the temperature variation of the unit-cell parameters for SrMo0.9Mg0.1O3−δ.", "The unit-cell parameters monotonically increase when heating the sample due to the expansion of the chemical bonds.", "The thermal evolution of the oxygen content in air was also studied by neutron diffraction.", "Figure 5b (right axis) illustrates the temperature variation of the oxygen vacancies concentration for SrMo0.9Mg0.1O3−δ.", "The oxygen content decreases when heating the sample in vacuum from SrMo0.9Mg0.1O2.985(3) for x = 0.1, almost stoichiometric at room temperature, to SrMo0.9Mg0.1O2.937(3) at 800 °C.", "As the sample is heated, the mixed-valence Mo4+-Mo5+ is reduced to Mo4+, generating oxygen vacancies.", "Figure 5b (left axis) shows the equivalent isotropic displacement factors of oxygen atoms (Beq) increasing from 0.81 at 25 °C to 2.34 Å2 at 800 °C.", "This feature, along with the presence of oxygen vacancies, indicates a high mobility of these atoms, allowing the required O2− motion across the three-dimensional network and providing the material with a good ionic conductivity at the working temperatures of an SOFC.", "For the cations (Sr, Mo, Mg), the thermal displacement parameters are constrained to be spherical.", "For O, the anisotropy of the thermal ellipsoids is patent, with the smallest thermal motions along the (Mo,Mg)-O bonds.", "The magnitude of the thermal motions is monotonically enhanced with temperature, as shown in Table 1.", "In the entire temperature regime, the O oblate ellipsoids, flattened along the Mo-O-Mo directions, are orientated along the [001] directions.", "Figure 6 shows the crystal structure of SrMo1−xMgxO3−δ highlighting the evolution of the anisotropic displacements between 200 and 800 °C, with 95% probability for the O nuclear density.", "At 800 °C, the root mean square (r.m.s.) displacements of O are 0.194 Å perpendicular to the Mo-Mo distance and 0.117 Å parallel to it.", "The disk-shaped ellipsoids are the result of the strong covalent bonding between Mo4+-Mo5+ and O; SrMoO3 is well known to exhibit band conduction properties by virtue of the robust covalent mixing between 4d Mo orbitals and O 2p oxygen orbitals, strongly overlapping across 180° Mo-O-Mo angles.", "Such strong chemical bonds impede the thermal motion along the bonds, in such a way that O atoms exhibit degrees of freedom in the plane perpendicular to the bonding direction.", "This is in contrast with the prolate ellipsoids observed in other MIEC oxides, like Ba0.9Co0.7Fe0.2Nb0.1O3−δ [13], which suggests a breathing of the (Co,Fe,Nb)O6 octahedra upon the migration of the oxygen vacancies across the solid.", "In that case, the average (Co,Fe) oxidation state varies between 2.84+ and 2.02+ in the 25–800 °C temperature range, thus involving much less covalent chemical bonds within the perovskite octahedra, which make possible the less-frequent prolate kind of thermal ellipsoids. 3.2.", "Thermal Analysis The oxidation of the samples by incorporation of oxygen was followed by thermogravimetric analysis carried out in O2 flow from 35–900 °C.", "Figure 7 shows the TGA curves for the SrMo1−xMgxO3−δ (x = 0.1 and 0.2) samples.", "The curves indicate an incorporation of 0.67 oxygen atoms per formula unit for the sample with x = 0.1 and 0.49 oxygens for x = 0.2.", "As the samples are heated, the oxidation of the perovskite compounds is produced, resulting in crystalline phases with a scheelite-type structure.", "The incorporation of the oxygen atoms occurs in the 350–500 °C temperature range.", "The Mo final valence after the oxidation is 5.71+ for x = 0.1 and 5.73+ for x = 0.2.", "Figure 8 shows the refined XRD pattern for the SrMo0.9Mg0.1O3.67 scheelite phase in the space group I41/a (No. 88) after thermogravimetric analysis in O2 flow.", "Sr atoms are situated at the 4b (0, 1⁄4, 5⁄8) position; Mo and Mg atoms are randomly distributed at 4a (0, 1⁄4, 1⁄8) sites; and O1 oxygen atoms are located at the 16f (x, y, z) position.", "The subsequent heat treatment of the oxidized scheelite phase in reducing (5% H2/95% N2) atmosphere restored the reduced perovskite phase, confirming the reversibility required in redox cycles.", "The scheelite structure is a superstructure of fluorite where all of the Mo ions are tetrahedrally coordinated to oxygen atoms, as shown in Figure 8b, with an ordered arrangement of Sr and Mo cations.", "The tetrahedral units are not connected, whereas the larger Sr cations show eight-fold coordination.", "A more accurate NPD study would be necessary to determine the oxygen occupancy and interatomic distances to Sr and Mo, in this potentially interesting oxygen-defective scheelite phase. 3.3.", "Thermal Expansion Measurements In order to probe the mechanical compatibility of our materials with the other cell components, thermal expansion measurements in dense samples were performed in a 5% H2/95% N2 atmosphere.", "The dilatometric analysis was carried out between 25 and 900 °C for several cycles; the data were only recorded during the heating process.", "Figure 9 shows the thermal expansion for SrMo1−xMgxO3–δ (x = 0.1 and 0.2) and SrMo1−xMgxO4–δ (x = 0.1 and 0.2).", "No abrupt changes in the entire temperature measuring range were found.", "TECs measured in 5% H2/95% N2 atmosphere for perovskite phases and an air atmosphere for scheelite phases between 400 and 850 °C are included in Figure 9.", "The TEC value for SrMo0.9Mg0.1O3−δ is in concordance with that obtained from NPD data in the heating run, of 10.93 × 10−6 K−1.", "The TECs obtained for the perovskite and scheelite phases are reasonably similar and fit with the general SOFC electrolytes values, so no mechanical compatibility problems should be expected during the oxidation-reduction cycles.", "For the x = 0.1 compound, the TEC coefficients for SrMo1−xMgxO3−δ and SrMo1−xMgxO4−δ are indeed very similar, exhibiting values of 11.74 × 10−6 and 11.23 × 10−6∙K−1, respectively.", "For x = 0.2, there is a bigger difference (10.64 × 10−6 and 13.94 × 10−6∙K−1, respectively), which could induce a certain redox instability. 3.4.", "Electrical Conductivity Measurements Figure 10 shows the thermal variation of the electrical conductivity of SrMo1−xMgxO3−δ (x = 0.1 and 0.2).", "The resistance was measured by the dc four-probe method; a current of 100 mA was applied, and the potential drop was recorded in an Autolab 302N Potentiostat-Galvanostat.", "Figure 10 illustrates the reduced phases with the perovskite structure featuring a metallic–like conductivity under reducing conditions in both cases.", "Figure 10 illustrates a clear reduction in the electrical conductivity when the Mg content increases, since Mg2+ perturbs the conduction paths via Mo-O-Mo chemical bonds, giving total conductivity values at the operating temperature (850 °C) of 146 and 114 S∙cm−1 for x = 0.1 and 0.2, respectively.", "These values are, in any case, sufficiently high for the correct performance of these materials as anodes in SOFC.", "For instance, σ values of 175 and 160 Scm−1 were described for SrMo0.9Fe0.1O3−δ [6] and SrMo0.9Cr0.1O3−δ [7] at 850 °C, showing an excellent performance in the hydrogen oxidation reaction in SOFC. 3.5.", "Chemical Compatibility The chemical compatibility of SrMo1−xMgxO3−δ series with La0.8Sr0.2Ga0.83Mg0.17O3−δ (LSGM) electrolyte has been studied by mixing of both powdered samples and heating the mixture at 900 °C under H2/N2 (5%/95%) atmosphere for 24 h.", "Figure 11 shows the Rietveld analysis of SrMo0.9Mg0.1O3−δ, consisting of a mixture of both unchanged phases, so no unwanted secondary phases will be formed during the operation in single cells.", "The same result was obtained for the compound with x = 0.2. 3.6.", "Fuel-Cell Tests In order to study the behavior of SrMo1−xMgxO3−δ (x = 0.1 and 0.2) as anodes in solid oxide fuel cells, a single cell for each sample was prepared in an electrolyte-supported configuration using a 300 μm-thick LSGM electrolyte, and the output power was measured at 800 and 850 °C.", "Figure 12 illustrates the cell voltage and power density as a function of current density at these temperatures for the single cell fed with pure H2 for the x = 0.1 anode.", "The maximum power densities generated by the cell were 684 and 887 mW/cm2, respectively.", "Figure 13 shows the cell voltage and power density as a function of current density at the same temperatures for the anode x = 0.2.", "The maximum power densities generated by the cell were 555 and 832 mW/cm2, respectively.", "The inset of Figure 13 illustrates a view of the cathode side of the cell.", "Although both anodes have an exceptional behavior, a slight decrease of the output power of the single cells is observed for x = 0.2 with respect to the x = 0.1 anode.", "This reduction of the power density could be related to the decrease in the Mo contents of the anode in the x = 0.2 sample, since apparently, molybdenum is responsible for the catalytic oxidation of the fuel, as has been observed in other Mo-containing anodes [6,14].", "Additionally, the observed reduction of the electrical conductivity (Figure 10) in the whole range of measured temperatures also contributes to the deterioration of the output power for this anode material.", "In a previous work [7], an additional test using Au gauze with a small amount of Au paste as the current collector instead of Pt gauze was carried out to check if Pt could promote the catalytic process of O2 reduction or fuel oxidation as suggested by some authors [15,16,17], increasing the power density and covering up the true activity of the oxides selected as electrodes.", "In this work, the maximum power densities generated by the cell were even higher than with Pt gauze.", "Since Au has no catalytic properties, this test implies that the observed activity comes entirely from the anode material.", "In order to compare the performance of our SrMo1−xMgxO3−δ (x = 0.1 and 0.2) anodes with other SrMo1−xMxO3−δ (M = Fe and Cr) anodes, in previous works [6,7], an identical single cell with these anodes was also made and measured.", "Similar power outputs were observed in these cases (874 mW/cm2 for SrMo0.9Fe0.1O3−δ and 695 mW/cm2 for SrMo0.9Cr0.1O3−δ at 850 °C), demonstrating that our anodes are even slightly better than these materials.", "Moreover, in the long-term performance, the Mg2+-doped anodes are believed to be superior due to the absence of interdiffusion cationic effects, since Mg is also contained in the LSGM electrolyte. 4.", "Conclusions In this study, we have shown that SrMo1−xMgxO3−δ (x = 0.1 and 0.2) oxides crystallize in a cubic perovskite structure (Pm-3m) where a mixed Mo4+-Mo5+ oxidation state is present at RT; NPD data unveil the creation of an appreciable amount of oxygen vacancies at high temperatures, under the low pO2 working conditions of an SOFC.", "The anisotropic displacements for O atoms, conforming flattened ellipsoids, correspond to the highly covalent Mo-O bonds.", "SrMo1−xMgxO3−δ (x = 0.1 and 0.2) oxides can be successfully used as anode materials in SOFC test cells in an electrolyte-supported configuration using a 300 μm-thick LSGM electrolyte.", "Excellent maximum output powers of 887 and 832 mW/cm2 are obtained for x = 0.1, 0.2, respectively, at 850 °C, using pure H2 as a fuel.", "The sufficiently large number of oxygen vacancies combined with high thermal displacement factors suggest a high ionic conductivity at the operating temperatures, constituting MIEC-type materials together with the high electronic conductivity associated with the pristine SrMoO3 sample.", "In addition, the reversibility of the reduction-oxidation between the Sr(Mo,Mg)O4−δ scheelite and Sr(Mo,Mg)O3−δ perovskite phases makes possible the required cyclability of the cells.", "The obtained TECs, ranging between 13.94 × 10−6 and 10.64 ×10−6 K−1, are perfectly compatible with the usual SOFC electrolytes.", "Finally, excellent chemical compatibility was observed with the electrolyte LSGM for 24 h at 900 °C." ]

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[ "Operation of Thin-Film Electrolyte Metal-Supported Solid Oxide Fuel Cells in Lightweight and Stationary Stacks: Material and Microstructural Aspects Operation of Thin-Film Electrolyte Metal-Supported Solid Oxide Fuel Cells in Lightweight and Stationary Stacks: Material and Microstructural Aspects RoehrensDaniel13*PackbierUte2FangQingping2BlumLudger2SeboldDoris1BramMartin13MenzlerNorbert1 IveyDouglas Academic Editor 1Forschungszentrum Jülich GmbH, Institute of Energy and Climate Research, IEK-1: Materials Synthesis and Processing, Jülich 52425, Germany; d.sebold@fz-juelich.de (D.S.); m.bram@fz-juelich.de (M.B.); n.h.menzler@fz-juelich.de (N.M.) 2Forschungszentrum Jülich GmbH, Institute of Energy and Climate Research, IEK-3: Electrochemical Process Engineering, Jülich 52425, Germany; u.packbier@fz-juelich.de (U.P.); q.fang@fz-juelich.de (Q.F.); l.blum@fz-juelich.de (L.B.) 3Christian Doppler Laboratory for Interfaces in Metal-Supported Electrochemical Energy Converters, Jülich 52425, Germany *Correspondence: d.roehrens@fz-juelich.de; Tel.: +49-2461-61-96650 762 In this study we report on the development and operational data of a metal-supported solid oxide fuel cell with a thin film electrolyte under varying conditions.", "The metal-ceramic structure was developed for a mobile auxiliary power unit and offers power densities of 1 W/cm2 at 800 °C, as well as robustness under mechanical, thermal and chemical stresses.", "A dense and thin yttria-doped zirconia layer was applied to a nanoporous nickel/zirconia anode using a scalable adapted gas-flow sputter process, which allowed the homogeneous coating of areas up to 100 cm2.", "The cell performance is presented for single cells and for stack operation, both in lightweight and stationary stack designs.", "The results from short-term operation indicate that this cell technology may be a very suitable alternative for mobile applications. metal-supported solid oxide fuel cell thin-film electrolyte stack operation gas-flow sputtering diffusion barrier layers 1.", "Introduction Materials science and engineering has been a major contributor to the progress of fuel cell technology [1].", "Especially, solid oxide fuel cells (SOFCs) have attracted a great deal of interest because of their fuel flexibility, versatility, and efficiency [2,3].", "The advancement of oxide ion electrolytes and the introduction of potent mixed ionic and electronic conducting (MIEC) electrodes has enabled a reduction in operating temperatures [4,5,6].", "This made it possible to incorporate metallic interconnects into the cell design at substantially lower costs than for their ceramic counterparts [7,8].", "Additionally, the development of materials and microstructures led to significant improvements in terms of power density and lifetime [9,10,11,12].", "However, production costs for conventional ceramic SOFCs and limited mechanical robustness remain limiting factors.", "Recent advances in powder-metallurgy have led to the establishment of another SOFC concept: the metal-supported SOFC (MSC) [13].", "Here, the electrochemically active ceramic cell is constructed on top of a porous, and usually highly corrosion-resistant, steel support.", "MSCs have been demonstrated to be a promising technology for operation under non-stationary conditions because of their comparatively high tolerance of thermal, mechanical, and chemical stresses [14,15].", "Additionally, the incorporation of standardized metal parts as a backbone permits relatively cheap mass manufacturing, which is crucial in terms of commercial competitiveness of the technology.", "In recent years, many different concepts have emerged enabling cheaper manufacturing and assembly, as well as increased mechanical stability [14,16,17,18,19,20,21,22,23,24].", "Of these, the Plansee SE’s cell design has gained considerable attention, since it is manufactured by a combined sintering and deposition route, leading to a very thin electrolyte membrane being realized [25,26,27].", "These cells have been manufactured on a pilot scale and achieve power densities comparable to their more mature ceramic SOFC counterparts [28].", "However, this type of metal-supported SOFC represents a much younger technology and previous electrochemical characterizations have been carried out mostly on a single-cell level or for symmetrical model samples.", "To our knowledge, results of electrical performance characterization and long-term testing in a stack environment has so far not been published.", "In this study, we summarize recent results with the Plansee SE MSC both in terms of electrical operation for single-cell arrangements, as well as for lightweight designs and in stationary stacks.", "Microstructural features before and after operation were explored with electron microscopy and energy dispersive X-ray spectroscopy. 2.", "Results and Discussion 2.1.", "Single-Cell Test Single-cell MSCs with small-area cathodes (1 cm2) have been characterized under various conditions [26].", "An example is given in Figure 1.", "This cell was activated in-situ for 10 h at 850 °C in a dual gas atmosphere (air/3% humidified hydrogen) in order to achieve densification and adhesion of the green La0.58Sr0.4Co0.2Fe0.8O3-δ (LSCF) cathode to the barrier layer.", "Although 10 h at 850 °C is not sufficient to ensure a sintering of the A-site-deficient LSCF cathode, the power densities obtained from single-cell tests with hydrogen are in a range that is comparable to full ceramic SOFCs (1.5 A/cm2 at 0.8 V and 850 °C).", "When the fuel gas is switched to a system-relevant simulated diesel reformate (50% N2, 15% H2 14% CO, 11% H2O, 10% CO2) and a temperature of 750 °C cell performances in the range of 200 to 630 mW/cm2 at 0.7 V were recorded [26], which is sufficient for the application of this type of cell in a mobile APU. 2.2.", "Lightweight Cassette Stack A two-layer lightweight stack was set up with cells welded into the interconnector frame.", "After the glass sealant crystallized during the joining process for 100 h at 850 °C, gas tightness was achieved.", "The fuel gas was then set to humidified hydrogen and galvanostatic stack operation commencing at 750 °C, 0.3 A/cm2, and a fuel utilization of 20%.", "The resulting I–V and performance curves are shown in Figure 2 and Figure 3.", "The measured IV-curves show a significantly reduced performance of the MSC (300 mA/cm2 at 0.8 V and 800 °C) as part of the stack compared to the single-cell measurements, both in terms of open circuit voltage (OCV) values and the slope of the voltage curve, which translates to a higher area-specific resistance.", "A lower OCV due to small internal leakages may be attributed to variations in the production cycle; the higher ASR compared to the single-cell test is a direct result of the introduction of several additional components which are necessary for stack operation, such as contacting oxide layers and or interconnector coatings.", "Due to the generally larger cell sizes, contact geometry and gas-flow are different compared to the single-cell laboratory experiment.", "Additionally, neighboring cells influence each other, for example with respect to temperature distribution [29].", "These factors may contribute to the earlier onset of transport limitation at a current density of about 0.8 A/cm2, thus explaining the difference to the single cell measurement.", "However, these issues are common when comparing single-cell experiments with stack operation and a performance loss of 30%–50% is observed frequently [30].", "In terms of performance degradation over time, the data indicate different behavior comparing cell 1 and cell 2 in Figure 2.", "While the cell voltage for cell 1 increases by 5.2 mV over 237 h of operation, which is probably a result of a slight improvement of the activity at the cathode side, cell 2 shows a progressive degradation of 18.62 mV or 2.4% over 237 h, which equates to 10.2% over 1000 h.", "This was, however, not related to intrinsic defects on the cell level, since OCV values for both cells were similar at 1.011 V (cell 1) and 1.015 V (cell 2) at 750 °C after the joining process, but rather were a direct result of an external leakage and subsequent reoxidation of cell 2 that developed during the course of the experiment, which resulted in an area increase in dark gray oxidized domains and some cracks in the cathode layer in the scanning electron microscopy (SEM) analysis.", "Cell 1, on the other hand, was subjected to less microstructural degradation, as can be seen in Figure 4a.", "A cross-section of cell 2 is presented in Figure 4b.", "Although the electrical performance of cell 1 did not show progressive degradation, an incipient corrosion of the metal substrate is visible as dark gray areas in Figure 4a (left).", "At the present time, it is unclear what the effect will be on the long term stability of the cell and the study of these issues is now part of research at the recently established Christian-Doppler Laboratory [31].", "The Ni/8YSZ, however, was not subjected to severe microstructural changes and the thin film electrolyte was found to be crack-free for the entire surveyed area.", "Additionally, the LSCF-cathode activated in situ shows good adherence to the electrolyte membrane and the porosity distribution was found to be homogeneous. 2.3.", "Stationary Stack In order to exclude influences characteristic of the lightweight stack design, an additional two-layer stack was set up according to a well-known stationary stack design.", "For this test, a higher, more system-relevant current density of 0.5 A/cm2 was selected.", "Before galvanostatic operation, an in situ activation of the cathode was conducted at 850 °C in dual gas conditions (air-side electrode: atmospheric air, fuel-side electrode: argon stream) for 100 h.", "After activation, IV curves were recorded with humidified hydrogen as fuel gas at different temperatures (see Figure 5).", "Both I-V curves show a significantly higher performance of the Plansee MSCs compared to the corresponding results from the lightweight stack (Figure 3).", "This is true for both cells from both stacks and can be explained by the improved electrical contact in the stationary design.", "Additionally, both cells in the stationary design show a higher OCV-value because of improved internal and external gas-tightness and a later onset of the gas-transport limitation, which is a result of a more efficient layout of the distribution manifolds and gas channels compared to the lightweight system.", "The initial cell characteristics, as shown in Figure 5, were very promising.", "However, during the operation of the stack elevated degradation was recorded (see Figure 6).", "Over the course of galvanostatic operation (43 h), cell 1 lost 31 mV or 4.15% of the initial value, while cell 2 degraded by 61 mV (8.31%).", "Although the rate of performance loss in Figure 6 decreased considerably with increasing time at 0.5 A/cm2, we decided to cool down the stack and investigate the cells’ microstructure.", "Representative cross-sections are shown in Figure 7.", "Although a slight internal leakage was detected after cooling down the stack, the thin 8YSZ electrolyte membrane was intact along the analyzed cross-sections (see Figure 7).", "No significant increase in local defect densities was observed compared to the initial state.", "Furthermore, the cathode microstructure and contact to the electrolyte were well established.", "EDS analysis of the cathode and electrolyte did not reveal any indications of a stoichiometric change in comparison to the as-prepared state.", "However, signs of progressive corrosion of the porous metal-support were found.", "The ITM substrate exhibited a large number of dark gray areas (see Figure 7, left), which were identified as Cr/Fe oxide phases by EDS analysis.", "These oxide areas are also found in direct contact with the Gd2O3-doped CeO2 (GDC) diffusion barrier, indicating insufficient inhibition of the cation transport under these conditions (see Figure 8).", "These interdiffusion phenomena may have been caused by insufficient stability of the barrier material GDC under the applied conditions.", "Indeed, it has been reported previously that doped cerates are prone to oxygen loss and phase transformation under highly reducing atmospheres, which enables interaction with neighboring materials or even decomposition [32].", "Higher performance degradation rates, compared to full ceramic SOFCs, are a relatively common phenomenon for MSCs and have been reported for various cell concepts by other groups [13,21,33,34,35].", "Reasons for this are in part the presence of the porous steel support, which may oxidize or coarsen during operation and can, at least in part, interact with the catalytically active centers of the anode (usually Ni).", "By applying a suitable and more redox-stable barrier layer, the expected lifetime of the MSC will increase significantly, while electrical properties remain largely unaffected. 3.", "Materials and Methods 3.1.", "Cell Design and Manufacturing The cell design is presented schematically in Figure 9.", "The first step in the production cycle is the manufacturing of the 0.8 mm thick porous metal support (Cr26-Fe, ITM) by a powder-metallurgical process.", "To avoid interdiffusion of Fe and Cr into the anode, the substrate is coated with a 500 nm thin Gd2O3-doped CeO2 (GDC) layer by magnetron sputtering.", "In the second step, a 40 μm multilayer nickel/8%-Y2O3-doped ZrO2 (Ni/8YSZ) anode is applied to the substrate by screen-printing and subsequently annealed in hydrogen atmosphere.", "The composition of the anode paste is varied in each step (finer particles, lower porosity) to ensure a graded improvement of the surface, which is necessary for the application of the 4 μm electrolyte membrane in step 3 via gas-flow sputtering (GFS).", "Finally, a 40 μm LSCF cathode is screen printed on top of a magnetron-sputtered 500 nm thin GDC diffusion barrier.", "Each step will be discussed in detail below. 3.1.1.", "Substrate The substrate (ITM) consists of an oxide dispersion-strengthened (OSD) ferritic steel containing 26% chromium, which is alloyed with small amounts of titanium, molybdenum, and Y2O3 additions.", "The material was prepared by a powder-metallurgical process and exhibits porosities of about 40%, good corrosion resistance and a thermal expansion coefficient that matches SOFC materials well and was found to be independent of the porosity [36,37,38].", "ITM was formed into sheets of 0.8 mm in thickness and different areas from 25 cm2 to 100 cm2, which can be welded to the interconnector frame.", "Figure 10 shows a cross-section and a fracture image, in which the oxide crystals along the grain boundaries are visible.", "The interdiffusion of cations from the metal substrate into the anode, and vice versa, can be a significant issue in the manufacturing and operation of MSCs and may lead to severe performance degradation [39].", "Fe and Cr, once transported into the anode, form alloys with the Ni-catalyst and, thus, reduce cell performance.", "A number of possible protective coatings for different steel supports displaying sufficient chemical stability, a matching thermal expansion coefficient (TEC), and electrical conductivity have been explored in the literature and shown to be effective [39,40,41].", "In this study we decided to produce a thin (0.5–1.0 μm) GDC layer by magnetron sputtering on top of the porous substrate, which is shown in Figure 11. 3.1.2.", "Fuel-Side Electrode In order to achieve a graded transfer from the large particle and pore sizes of the ITM substrate, a 3-step screen-printing process was developed.", "In contrast to the manufacturing of full ceramic SOFCs, which relies on atmospheric sintering of NiO, the screen printing pastes for the Plansee MSC are based on metallic Ni particles.", "To avoid high-temperature corrosion of the metal substrate, sintering has to be conducted in reducing atmosphere and anode porosities have to be defined by the organic content of the paste.", "Sintering is conducted at 1180 °C in hydrogen atmosphere.", "By gradually reducing the particle size of Ni in the screen-printing pastes and adjusting the solid load, composition and paste rheology a very smooth and homogeneous surface was achieved, which is necessary for the successful application of a thin 8YSZ electrolyte by gas-flow sputtering.", "A cross-section image of a sintered 3-layer anode is presented in Figure 12. 3.1.3.", "Electrolyte Membrane Dense and thin (4 μm) 8YSZ electrolytes have been prepared on top of the graded Ni/8YSZ anode by means of a gas-flow sputter process for active areas of up to 84 cm2.", "This method allows high deposition rates and a wide range of possible compounds and is generally considered to be a more economic physical vapor deposition (PVD) method [42].", "After GFS processing, the 8YSZ membrane shows a low defect density and leakage rates of less than 3 × 10−4 hPa·dm3·s−1·cm−2 (Δp: 100 hPa) in air at room temperature have been obtained, which is sufficient for the electrical operation of the cell [27].", "The 8YSZ layer adheres well to the anode surface and is able to withstand small height variations of the support even after operation (see Figure 13).", "Additionally, it was found that the thin membrane is flexible with respect to mechanical stresses which may arise from the oxidation of the anode or variations in thermal expansion coefficients [43].", "This is a phenomenon which is characteristic of thin membranes, in general, and was recently reported for full ceramic SOFCs [44].", "Due to the reactivity of the LSCF cathode material with zirconia, a dense 500 nm GDC layer is deposited by magnetron sputtering on top of the electrolyte in a second step to avoid the formation of strontium zirconates, which are detrimental to cell performance [45]. 3.1.4.", "Air-Side Electrode Cathodes 40 μm in thickness were applied by screen printing on top of the electrolyte/diffusion barrier layer.", "Sr- and Fe-doped lanthanum cobaltites, in general, and A-site-deficient LSCF, in particular, have been used for SOFCs of all kinds and lead to excellent cell performance [46,47].", "However, due to the presence of the metal substrate, a conventional sintering route at temperatures higher than 1000 °C in air is not possible for the MSC.", "Due to this, the cathode was kept in its green state during stack assembly and the first heat-up of the cell.", "An in situ activation step (850 °C, 10 to 100 h) in dual gas conditions was applied in order to ensure sufficient adherence to the electrolyte and, thus, good cell performance.", "The microstructure of the cathode after this activation step is shown in Figure 13 in Section 3.1.3. 3.1.5.", "Stack Assembly Two MSCs with an active area of 84 cm2 each were assembled into a lightweight cassette design that was developed for a mobile APU.", "The setup has been published earlier [26] and will only be discussed briefly.", "The interconnector frame was made up of dense ITM and accommodates the gas distribution manifolds.", "High temperature sealing was accomplished by using a conventional glass-ceramic [48].", "During the joining process, the two-layer short stack was heated to 850 °C for 100 h in a dual gas atmosphere under a mechanical load of 0.5 kN.", "After that, the temperature was set to 750 °C and stack operation commenced under constant current conditions (0.3 A/cm2).", "In addition to the lightweight setup, 10 × 10 cm2 MSCs were incorporated into a stack that was developed for stationary applications.", "Details can be found in a previous publication [29].", "The joining process was identical to the lightweight-stack.", "Electrical operation was conducted galvanostatically at a lower temperature (700 °C) and under higher current density (0.5 A/cm2), compared to the lightweight setup, in order to expose the MSCs to conditions that were more relevant to the system’s point of operation.", "For both stacks, humidified hydrogen was supplied to the fuel-side electrode (cassette stack Uf = 20%, stationary-stack Uf = 40%). 3.1.6.", "Electron Microscopy The SEM (scanning electron microscopy) images of polished cross sections were taken using a Zeiss Ultra55 (Oberkochen, Germany) with INCA Energy 355 EDX (energy-dispersive X-ray) and INCA Crystal EBSD (electron backscatter diffraction) detectors. 4.", "Conclusions A metal-supported SOFC based on a porous steel substrate, a graded three-layer Ni/8YSZ anode, and a thin film 8YSZ membrane was operated in two different stack designs.", "The cells were characterized in terms of electrical performance and microstructural behavior.", "Single cell IV-characterization of such cells with an LSCF cathode activated in situ displays power densities of about 1 W/cm2 at 800 °C and 1.5 A/cm2.", "A two-layer lightweight MSC stack with an 84 cm2 active cell area was operated at 0.3 A/cm2 for more than 237 h at 750 °C.", "IV characterization of the cells activated in situ showed a reduction of the power densities obtained due to contacting and gas-transport losses, which is in line with other studies.", "A further two layer MSC stack in a stationary design was set up and operated at 0.5 A/cm2 for 43 h.", "For both stacks, one cell each showed increased degradation rates, while the other one remained relatively stable.", "The increased degradation rate is at least in part the result of setup related issues, which was confirmed by post-test microstructural analysis of the cells.", "Even though cell degradation for this MSC concept was higher compared to traditional full ceramic SOFCs, the first results from stack operation show performance data that are sufficient for the operation of a mobile APU, while a future redesign of current diffusion barrier layers will contribute greatly to extending cell lifetime." ]

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[ "Rational Design of a Water‐Storable Hierarchical Architecture Decorated with Amorphous Barium Oxide and Nickel Nanoparticles as a Solid Oxide Fuel Cell Anode with Excellent Sulfur Tolerance Rational Design of a Water‐Storable Hierarchical Architecture Decorated with Amorphous Barium Oxide and Nickel Nanoparticles as a Solid Oxide Fuel Cell Anode with Excellent Sulfur Tolerance SongYufei 1 WangWei http://orcid.org/0000-0001-7496-4548 2 GeLei 3 XuXiaomin http://orcid.org/0000-0002-0067-3331 2 ZhangZhenbao 1 JuliãoPaulo Sérgio Barros 2 ZhouWei http://orcid.org/0000-0003-0322-095X zhouwei1982@njtech.edu.cn 1 ShaoZongping http://orcid.org/0000-0002-4538-4218 shaozp@njtech.edu.cn 2 4 1 State Key Laboratory of Materials‐Oriented Chemical Engineering College of Chemical Engineering Jiangsu National Synergetic Innovation Center for Advanced Materials (SICAM) Nanjing Tech University No. 5 Xin Mofan Road Nanjing 210009 P.", "R.", "China 2 Department of Chemical Engineering Curtin University Perth Western Australia 6845 Australia 3 Center for Future Materials University of Southern Queensland Springfield Central Queensland 4300 Australia 4 State Key Laboratory of Materials‐Oriented Chemical Engineering School of Energy Science and Engineering Jiangsu National Synergetic Innovation Center for Advanced Materials (SICAM) Nanjing Tech University No. 5 Xin Mofan Road Nanjing 210009 P.", "R.", "China *E‐mail: zhouwei1982@njtech.edu.cn, shaozp@njtech.edu.cn 10.1002/advs.v4.11 1700337 Abstract Solid oxide fuel cells (SOFCs), which can directly convert chemical energy stored in fuels into electric power, represent a useful technology for a more sustainable future.", "They are particularly attractive given that they can be easily integrated into the currently available fossil fuel infrastructure to realize an ideal clean energy system.", "However, the widespread use of the SOFC technology is hindered by sulfur poisoning at the anode caused by the sulfur impurities in fossil fuels.", "Therefore, improving the sulfur tolerance of the anode is critical for developing SOFCs for use with fossil fuels.", "Herein, a novel, highly active, sulfur‐tolerant anode for intermediate‐temperature SOFCs is prepared via a facile impregnation and limited reaction protocol.", "During synthesis, Ni nanoparticles, water‐storable BaZr0.4Ce0.4Y0.2O3− δ (BZCY) perovskite, and amorphous BaO are formed in situ and deposited on the surface of a Sm0.2Ce0.8O1.9 (SDC) scaffold.", "More specifically, a porous SDC scaffold is impregnated with a well‐designed proton‐conducting perovskite oxide liquid precursor with the nominal composition of Ba(Zr0.4Ce0.4Y0.2)0.8Ni0.2O3− δ (BZCYN), calcined and reduced in hydrogen.", "The as‐synthesized hierarchical architecture exhibits high H2 electro‐oxidation activity, excellent operational stability, superior sulfur tolerance, and good thermal cyclability.", "This work demonstrates the potential of combining nanocatalysts and water‐storable materials in advanced electrocatalysts for SOFCs. anode energy conversion solid oxide fuel cells sulfur tolerance water‐storable material National Natural Science Foundation of China 21576135 Youth Fund of Jiangsu Province BK20150945 Priority Academic Program Development of Jiangsu Higher Education Institutions Australian Research Council Discovery Projects program DP150104365 and DP160104835 source-schema-version-number 2.0 component-id advs411 cover-date November 2017 details-of-publishers-convertor Converter:WILEY_ML3GV2_TO_NLMPMC version:5.2.6.1 mode:remove_FC converted:23.11.2017 Y.", "Song , W.", "Wang , L.", "Ge , X.", "Xu , Z.", "Zhang , P.", "S.", "B.", "Julião , W.", "Zhou , Z.", "P.", "Shao , Adv.", "Sci. 2017, 4, 1700337 https://doi.org/10.1002/advs.411 A useful strategy for a cleaner, more sustainable future is to improve the energy conversion efficiency of fossil fuels with minimized emissions.", "Fuel cell technology enables chemical energy stored in the fuels to be converted to electric power via an electrochemical route that is not limited by the Carnot cycle, thus ensuring high efficiency.1, 2, 3 Furthermore, the exhaust gas is not diluted by N2, which would make subsequent CO2 sequestration easier and therefore results in a decrease in the greenhouse gas emissions.", "Among the various types of fuel cells, solid oxide fuel cells (SOFCs) are particularly attractive because they can be easily integrated into currently available fossil fuel infrastructure to obtain an ideal clean energy system.4, 5, 6, 7 To realize their widespread use, however, some important issues must be resolved.", "Because fossil fuels contain sulfur impurities, even after the purification, the anode must exhibit high sulfur tolerance.", "H2S concentrations as low as a few ppm can cause a dramatic decrease in the performance of cells with conventional Ni‐based cermet anodes.8 Due to the low activation energy of H2S dissociation at these anodes, sulfur atoms are easily generated and block the active sites on the Ni surface, thereby inhibiting the fuel oxidation.9 Therefore, improving the anode sulfur tolerance is critical for developing SOFCs for use with fossil fuels.", "Over the past decade, much research has been focused on developing new materials and architectures, such as Ni alloys with sulfur‐tolerant elements, oxide electrodes, anode functional layers, unique anode architectures, and nanocatalyst‐modified anode surfaces,10, 11, 12, 13, 14 for improving the sulfur tolerance of SOFC anodes.", "However, none of the tested systems meets all the strict requirements for practical SOFC anodes, such as good compatibility with other cell components, high conductivity, high fuel electro‐oxidation/reforming activities and excellent coking/sulfur resistance.", "For example, the introduction of a sulfur‐tolerant metal decreased the electro‐oxidation activity of the anode, whereas the oxide‐based anodes suffer from poor electronic conductivity and electro‐oxidation activity at low temperatures.", "To date, extensive studies have shown that Ni is the preferred electrocatalyst for fuel electro‐oxidation in SOFCs due to its superior activity, conductivity, and thermal compatibility.15, 16 However, this catalyst must be modified to enable its direct use with fossil fuels.", "One important modification strategy is to decrease the Ni particle size to nanometer scale to improve the interaction between Ni and substrate.17, 18, 19 Exsolution of Ni‐based nanoparticles from a perovskite lattice under reducing conditions at high temperatures is a promising approach to preparing ultrafine Ni‐based nanoparticles with excellent coking/sulfur tolerance and activity.18, 19 However, this strategy usually produces a limited number of Ni‐based nanoparticles.", "Very recently, Du et al. reported the fabrication of an Sr3FeMoO7− δ and SrFexMo1− xO3− δ composites decorated with FeNi3 alloy nanoparticles by reducing the Sr2FeMo0.65Ni0.35O6− δ double perovskite oxide at a high temperature, showing favorable activity and high coking resistance.20 The number of Ni–Fe alloy nanoparticles deposited on the composite was high due to the conversion‐type reaction used to prepare it.", "However, the thermal compatibility of this anode with other cell components remains a major concern because the phase transition that occurred during reduction might induce considerable thermal expansion.", "Another important strategy for improving the coking/sulfur tolerance of Ni‐based anodes is to increase the gasification rate of deposited carbon/sulfur on the anode.21, 22, 23 In the oxygen‐ion‐conducting SOFCs, water is produced at the anode under current polarization, which can be used to remove the deposited carbon/sulfur on the anode.", "In a pioneering work, Liu and co‐workers reported that BaO nanoparticles deposited on Ni surface can adsorb water, facilitating the rapid removal of the deposited carbon/sulfur on the anode.21 More recently, Shao and co‐workers demonstrated that using a water‐storable proton conductor in a Ni‐based anode resulted in excellent coking/sulfur resistance.22, 23 However, the operational stability of this anode was unsatisfactory due to the large Ni particle size and poor contact between Ni and the water‐storable phase.23 Due to the complexity of the electrode reactions at SOFC anodes, it is difficult to simultaneously achieve high electro‐oxidation activity and good coking/sulfur tolerance by a single strategy; therefore, a combination of various strategies is desirable.", "Herein, we prepared a novel, highly active, sulfur‐tolerant SOFC anode by a facile impregnation and limited reaction protocol.", "First, a proton‐conducting perovskite oxide with a nominal composition Ba(Zr0.4Ce0.4Y0.2)0.8Ni0.2O3−δ (BZCYN) was designed and then introduced into a porous SDC scaffold by impregnation, followed by calcination.", "Then, a limited reaction was performed by H2 treatment at 800 °C to obtain a porous hierarchical architecture consisting of Ni nanoparticles, water‐storable BaZr0.4Ce0.4Y0.2O3−δ (BZCY) perovskite and amorphous BaO deposited on SDC scaffold.", "The obtained anode exhibited excellent sulfur tolerance, H2 electroactivity, durability, and thermal cyclability at intermediate temperatures.", "This work opens a new avenue for the rational design of SOFC anodes with great potential in practical applications.", "The capability of Ni doping into BZCY perovskite lattice by synthesis under oxidizing atmosphere and Ni exsolution from the perovskite lattice under reducing atmosphere was first confirmed by X‐ray diffraction (XRD).", "As shown in Figure S1 in the Supporting Information, crystalline NiO phase was not detected in the as‐synthesized BZCYN sample.", "Instead, a pure cubic perovskite structure with a lattice parameter of 4.292 Å, which is slightly smaller than that of Ni‐free BZCY (4.302 Å), was observed.", "The smaller BZCYN lattice parameter is consistent with the fact that the ionic radius of Ni2+ (0.69 Å) is smaller than those of Zr4+ (0.72 Å), Ce4+ (0.87 Å), Ce3+ (1.02 Å), and Y3+ (0.90 Å).", "The decrease in the lattice parameter and absence of NiO crystalline phase strongly indicated that Ni was successfully doped into BZCYN perovskite lattice.", "After H2 treatment, a weak metallic Ni peak appeared, indicating successful Ni exsolution from the perovskite lattice.", "Moreover, the lattice parameter of the main perovskite phase increased to 4.310 Å, possibly due to Ni exsolution and Ce4+ partial reduction (Figure S2, Supporting Information).", "The successful Ni exsolution from the perovskite lattice after H2 treatment was further confirmed by Ni 2p X‐ray photoelectron spectroscopy (XPS) in Figure 1 a.", "Before reduction, the Ni 2p peaks of BZCYN sample were observed at 858.0 and 864.0 eV, indicating the presence of Ni2+.", "After H2 treatment, Ni2+ peaks disappeared and new Ni0 peaks appeared at 856.2 and 863.0 eV.", "Interestingly, XPS survey spectra show that the Ba atomic percentage of BZCYN surface increased from 40.0 to 47.0 at% after H2 treatment (Figure 1b), suggesting that Ni exsolution was accompanied by BaO surface enrichment.", "Therefore, the following reaction was proposed to occur in H2 treatment: Ba(Zr0.4Ce0.4Y0.2)0.8Ni0.2O3− δ + 0.2H2 → 0.8BaZr0.4Ce0.4Y0.2O3− δ + 0.2BaO + 0.2Ni + 0.2H2O.", "The absence of BaO crystalline phase peaks in the XRD pattern revealed its amorphous nature.", "Because the dissolution of free BaO occurs more readily in water than Ba2+ leaching from BZCYN perovskite lattice, the Ba2+ concentration of the reduced BZCYN soaking water was much higher than that of the as‐synthesized BZCYN soaking water (125 vs 54 ppm), verifying the formation of BaO phase.", "Although the perovskite structure can tolerate a large A‐site cation deficiency, a B‐site cation deficiency is usually energetically unfavorable.24 Ni exsolution from BZCYN during H2 treatment resulted in the formation of B‐site cation‐deficient perovskite, which promoted Ba leaching from the perovskite lattice.", "Figure 1 XPS a) Ni 2p and b) survey spectra of as‐synthesized and reduced BZCYN anodes.", "The Ba, Zr, Ce, Y, and Ni atomic percentages are shown in the inset.", "SEM images of c) as‐synthesized and d) reduced BZCYN anodes, e) STEM‐EDX results, f) TEM images and g) corresponding EDX results for the reduced BZCYN anode.", "The morphologies and phase compositions of the as‐synthesized and reduced BZCYN were examined by scanning electron microscopy (SEM), high‐resolution transmission electron microscopy (HR‐TEM) and scanning transmission electron microscopy (STEM) combined with energy‐dispersive X‐ray (EDX) spectroscopy.", "The as‐synthesized BZCYN surface was smooth (Figure 1c), whereas many nanoparticles with an average size of ≈25 nm (Figure 1d; Figure S3, Supporting Information) were observed on reduced BZCYN surfaces.", "Figure 1e shows that the large grains of reduced BZCYN were composed of Ba, Zr, Ce, and Y elements, whereas the nanoparticles were composed of Ni.", "Figure 1f shows that the reduced BZCYN sample consisted of two components: large, dark particles and lighter nanoparticles on their surfaces.", "The HR‐TEM and EDX results further confirmed that the nanoparticles and large grains were metallic Ni and BZCY perovskite phase, respectively (Figure 1f,g).", "The nanoparticle and main phase interplanar spacings of 0.202 and 0.181 nm were assigned to metallic Ni (111) and BZCY (211) planes, respectively.", "Interestingly, the nanozone (Region 2) in Figure 1f did not exhibit a lattice structure, suggesting that it was amorphous BaO in combination with the EDX results.", "The composition and morphology of the electrode fabricated by the impregnation and limited reaction method was also characterized (Figures S4–S7, Supporting Information).", "Again, the successful Ni doping into the perovskite lattice was confirmed by the decrease in the lattice parameter and the uniform distribution of Ba, Zr, Ce, Y, and Ni in BZCYN sample (Figures S4–S6, Supporting Information).", "The SDC scaffold displayed a highly porous architecture, built from well‐distributed particles with the size of 200–400 nm (Figure S7a, Supporting Information).", "After impregnating the porous SDC scaffold with BZCYN phase and then calcining it, its walls were decorated with many BZCYN nanoparticles with the size of 100 nm (Figure S7b, Supporting Information).", "After further treatment with H2, some even smaller nanoparticles with the size of ≈30 nm appeared on the surface of the impregnated perovskite phase, which were assigned to the metallic Ni phase (Figure S7c, Supporting Information).", "The phase structure and morphology of the thin porous layer on the SDC scaffold surface (Figure S8, Supporting Information) were similar to those of the reduced BZCYN powder (Figure 1d–g), suggesting that the compositional and morphological investigation of the reduced BZCYN powder could provide insight into the structures of the reduced BZCYN‐infiltrated SDC anode.", "Thus, the dark nanoparticles (≈30 nm in size), lighter particles, and amorphous region were assigned to Ni, BZCY, and BaO phases, respectively (Figure S8, Supporting Information).", "Figure S9 in the Supporting Information shows that the limited reduction reaction, during which the Ni nanoparticles and amorphous BaO phase were formed, led to a simultaneous increase in the pore volume and Brunauer–Emmett–Teller (BET) surface area.", "More specifically, the BET surface area of BZCYN increased from 4.58 to 7.77 m2 g−1 after H2 reduction.", "The total pore volumes of the BZCYN and reduced BZCYN were 0.019 and 0.039 mL g−1, respectively.", "The porous nature of the reduced BZCYN layer might facilitate gas diffusion, and the enlargement in the surface area increased the triple phase boundary (TPB) length.", "Both of these changes are advantageous for fuel oxidation at the electrode.", "Figure 2 a–f shows the 3D surface‐rendered image of the individual phases (SDC, BZCYN, and pores) in the BZCYN‐infiltrated SDC anode based on focused ion beam SEM (FIB‐SEM) images (Figure S10, Supporting Information).", "The individual phases were separated by image thresholding.", "The BZCYN dispersion in the infiltrated anodes was significantly enhanced after reduction, as shown by more numerous and smaller particles (Figure 2g,h).", "The enhanced catalyst dispersion due to the increased pore volume after H2 treatment should result in an increase in the number of active sites or the TPB length and thus enhance the electroactivity of the electrode.", "Figure 2 3D surface‐rendered image obtained from the segmented FIB‐SEM tomograms of the BZCYN‐infiltrated SDC anodes before (left) and after (middle) reduction in H2: a,b) SDC, c,d) BZCYN, e,f) voids.", "BZCYN particle size distributions (right) derived from image analysis of the FIB‐SEM tomogram g) before and h) after reduction in H2.", "To demonstrate the potential of this unique electrode architecture as an SOFC anode, several cells with different anodes were fabricated, and their electrochemical performances were compared.", "A cell with reduced BZCYN anode delivered a peak power density (PPD) of 184 mW cm−2 at 800 °C operating on H2, which was 3.6 times that of a cell with Ni‐free BZCY anode, indicating the importance of the exsolved Ni phase for H2 electro‐oxidation reaction (Figure S11a, Supporting Information).", "Specifically, this phase improves both the electronic conductivity and catalytic activity of the anode.", "A cell consisting of reduced BZCYN‐infiltrated SDC anode, thick SDC electrolyte and Ba0.5Sr0.5Co0.8Fe0.2O3− δ + SDC cathode (Figure S12, Supporting Information) with the thicknesses of ≈30, 300, and 20 μm, exhibited PPDs of 590, 535, 458, 369, and 297 mW cm−2 operating on H2 fuel at 800, 750, 700, 650, and 600 °C, respectively (Figure S11b, Supporting Information).", "These high power outputs are remarkable considering the thickness of the electrolyte (300 μm).", "The much higher power output of the cell with BZCYN‐infiltrated SDC anode compared with the cell with BZCYN anode indicates that the electrode microstructure significantly affects the H2 electro‐oxidation reaction.", "Furthermore, the use of the SDC scaffold effectively increased the TPB length by extending the reaction region to encompass most of the electrode.", "Figure 3 a shows that the PPDs of the cells with reduced BZCYN‐ and Ni‐infiltrated SDC anodes were 590 and 464 mW cm−2 operating on H2, respectively, indicating that H2 electro‐oxidation was promoted by the BZCY phase.", "When the fuel was 200 ppm H2S in H2, the PPDs and electrode polarization resistances of the cell with the reduced BZCYN‐infiltrated SDC anode were similar to those obtained with H2 fuel (Figure 3b; Figure S13, Supporting Information), demonstrating the excellent sulfur tolerance of this anode.", "Figure 3b shows that when the fuel was 200 ppm H2S in H2, the PPDs of the cells with the reduced BZCYN‐infiltrated SDC, Ni‐infiltrated SDC, and BZCY‐infiltrated Ni+SDC anodes were 561, 424, and 381 mW cm−2, respectively, which corresponds to decreases of 4.9%, 8.6%, and 13.2% relatively to those obtained with pure H2.", "These results demonstrated the superior sulfur tolerance of the reduced BZCYN‐infiltrated SDC anode, which was further confirmed by the differences in the electrode polarization resistances (Figure S14, Supporting Information).", "As shown in Figure S14 in the Supporting Information, it was found that there were some differences in the ohmic resistances, which could be attributed to the reconstruction, diffusion, and loss of the Ni active sites in the Ni‐infiltrated SDC and BZCY‐infiltrated Ni+SDC anodes.23, 25 Due to the strong water‐storage capability of amorphous BaO and BZCY proton conductor in the reduced BZCYN‐infiltrated SDC anode, the deposited sulfur on the anode surface can be rapidly eliminated, which can prevent the formation of nickel sulfides (Ni2S3) on the Ni surface.", "However, due to the poor sulfur tolerance of the Ni‐infiltrated SDC and BZCY‐infiltrated Ni+SDC anodes, the sulfur adsorbed on Ni surface cannot be eliminated immediately, resulting in the formation of Ni2S3, which was easily to be dissociated at 800 °C since its melting point was only 787 °C.5 As a result, the dissolution of Ni2S3 led to the continuous reconstruction, diffusion, and loss of Ni in the anode, which may cause the large differences in the ohmic resistances of the cells with different infiltrated anodes.", "Figure 3 I–V curves for SOFCs with different infiltrated anodes obtained using a) H2 and b) 200 ppm H2S in H2 at 800 °C.", "Stability tests for SOFCs with reduced BZCYN‐ and Ni‐infiltrated SDC anodes obtained with c) 200 and d) 100 ppm H2S in H2 at 800 °C.", "In addition to the power density, the operational stability of the electrode is also critical for practical applications.", "Figure 3c,d shows that the voltage of the cell with the reduced BZCYN‐infiltrated SDC anode remained nearly constant at 0.7 V for 24 and 50 h in 200 and 100 ppm H2S–H2 fuels, respectively.", "In contrast, the voltages of the cells with Ni‐infiltrated SDC anode rapidly decreased with time on stream.", "For practical application, the fuel cell may be required multiple start‐up and shut‐down operations in its whole lifetime, thus a high thermal stability and thermomechanical compatibility of the cell is required.", "The cell was heated up to 700 °C in H2 at a rate of 10 °C min−1 and holding for 20 min to achieve stable open‐circuit voltage (OCV) and PPD, and then the cell was cooled down to 200 °C in H2 at a rate of 2 °C min−1.", "The effect of thermal cycling on the anode stability was monitored by the power output of the fuel cell as shown in Figure S15 in the Supporting Information.", "The OCV and PPD of the single cell were well maintained at 0.88 V and 360 mW cm−2 in the 14 cycles involving the quick heating‐up and cooling‐down procedures, suggesting the superior thermal cyclability of the reduced BZCYN‐infiltrated SDC anode.", "For the infiltrated anodes, the thermal expansion behavior is very close to the electrolyte, which ensured the long‐term stability of SOFCs.", "As shown in Figure S16 in the Supporting Information, the thermal expansion coefficient (TEC) value of the SDC scaffold was 12.4 × 10−6 K−1, which agrees well with that reported in the literature.26 A little lower TEC value of 11.4 × 10−6 K−1 was obtained for the reduced BZCYN‐infiltrated SDC anode in comparison with the fresh one (12.6 × 10−6 K−1), which could be attributed to the formation of Ni nanoparticles and amorphous BaO in the reduction process.", "It suggested the reduced BZCYN‐infiltrated SDC anode was highly compatible with SDC electrolyte, such good thermomechanical compatibility ensures a good operational stability.", "It is well known that the electrode reaction usually appears at the region of TPB where the electrolyte (oxygen‐ion‐conducting phase), the electrode (electronic‐conducting phase), and the gas phase meet.", "An increase in the TPB length will provide larger number of active reaction sites, thus an improvement in electrode performance is expected.", "Because of the high ionic conductivity of SDC, the oxygen‐conducting phase was successfully penetrated into the electrode layer by applying the SDC scaffold.", "As a result, the TPB length is effectively increased by extending the reaction region into the bulk of electrode.", "Besides, the formation of porous structure from the limited conversion reaction exposed more active sites to surrounding atmosphere, thus the TPB length was further increased.", "It indicates that the building of the special hierarchical porous architecture through impregnation and limited conversion reaction greatly increased the TPB length, thus contributing to the superior electrocatalytic activity for H2 oxidation.", "In addition to the TPB length, the electrochemical activity of an electrode for fuel oxidation is also closely related to its intrinsic activity.", "It is well demonstrated that the reduction of particle size to the nanometer range can introduce some unusual properties, such as boosting the catalytic activity.", "In particular, recently, it was demonstrated that nickel nanoparticles showed outstanding performance for fuel electro‐oxidation.27, 28, 29 Clearly, the creation of abundant nickel nanoparticles from the limited conversion reaction of BZCYN further improved the electrode performance for H2 electro‐oxidation for power generation.", "Typically, nickel is easily poisoned by sulfur due to the easy adsorption of sulfur on the nickel surface for the low H2S dissociation energy.", "The sulfur adsorption over the nickel surface will block the catalytic reaction for fuel electro‐oxidation.", "As a result, a quick deterioration for the conventional nickel‐based electrode performance may be experienced when a small amount of sulfur was presented in the fuel gas.", "Sulfur poisoning can be reduced by two different strategies: changing the Ni electronic structure or increasing the rate of sulfur removal from the Ni surface.", "The electronic structure of Ni can be altered by alloying or changing the interaction between Ni and the substrate.", "As shown in Figure S17 in the Supporting Information, the onset temperature and peak temperature are two most important parameters to embody the easiness of the reduction of NiO, which are closely related to the NiO‐substrate interaction.", "The NiO was reduced at an onset temperature of around 203 °C, and the peak temperatures were 260 and 351 °C, which matched pretty well with the literature.22 For the NiO+SDC anode, the onset temperature and the peak temperature were found to be 280 and 409 °C, respectively, which were comparable to those of the free NiO, respectively, suggesting the weak interaction between NiO and SDC in the conventional NiO+SDC anode.", "As to the BZCYN‐infiltrated SDC, a reduction onset temperature of 300 °C and peak temperatures of 396 and 615 °C were derived from the hydrogen temperature‐programmed reduction (H2‐TPR) profiles, suggesting the BZCYN‐infiltrated SDC anode showed stronger Ni‐substrate interaction compared to the NiO+SDC anode, which could contribute to its superior sulfur tolerance by reducing sulfur adsorption (Figure S17, Supporting Information).", "In addition, sulfur poisoning can be reduced by gasifying the deposited/adsorbed sulfur on the anode.", "The reduced BZCYN anode could store more water than Ni+SDC anode due to the presence of BZCY and amorphous BaO phases (Figure S18, Supporting Information).", "A water desorption peak was observed from an onset temperature of 55 °C and peaked at 107 and 293 °C, suggesting the BZCYN was water storable.", "This is well understood since both BZCYN and BZCY are proton conductors, and the amorphous BaO also contributed to the water storage.", "For comparison, the conventional Ni+SDC anode showed almost no water‐storage capability.", "The superior sulfur tolerance of the reduced BZCYN‐infiltrated SDC anode was probably due to both the enhanced Ni‐substrate interaction and higher water‐storage capacity.", "Based on the above analysis, the superior performance of the SOFC anode modified with amorphous BaO and Ni nanoparticles could be explained by the mechanism shown in Figure 4 .", "First, H2 fuel is oxidized from the cathode at TPB to generate water (Equation (1)), and sulfur simultaneously adsorbed on Ni surface to form a surface‐adsorbed sulfur species ( S Ni ∗ ) (Equation (2)).", "Water is subsequently stored in BZCY by (OH)o formation (Equation (3)).", "Meanwhile, water is also physically adsorbed on amorphous BaO surface (Equation (4)).", "Then, the (OH)o species and physically adsorbed water can react with ( S Ni ∗ ) to generate SO2 and H2.", "Finally, SO2 desorbs from the Ni surface (Equations (5) and (6)), whereas H2 is oxidized to form H2O (1) H 2 + O 2 − → H 2 O + 2 e − (2) H 2 S + Ni → S Ni * + H 2 (3) H 2 O + O o × + V o • • → 2 OH o • (4) BaO + H 2 O → Ads H 2 O on BaO (5) S Ni * + 2 OH o • + 2 e – → SO 2 + H 2 (6) S Ni * + 2 Ads H 2 O on BaO → SO 2 + 2 H 2 Figure 4 Proposed mechanism for water‐induced sulfur removal from the hierarchically structured anode modified with Ni nanoparticles and amorphous BaO.", "In summary, a highly active, sulfur‐tolerant, water‐storable anode was successfully fabricated by impregnation, followed by calcination and a limited reaction.", "This anode had a hierarchical structure that was modified with amorphous BaO and Ni nanoparticles.", "It exhibited excellent chemical and thermal compatibility with the other cell components, good sulfur tolerance, high electro‐oxidation activity, and excellent thermomechanical stability.", "The cell constructed with this anode exhibited better stability in the H2S–H2 fuel than that with a conventional Ni+SDC anode, due to the stronger Ni‐substrate interaction and higher water‐storage capacity.", "This work demonstrated a novel, effective approach for developing sulfur‐tolerant SOFC anodes, which can accelerate the commercialization of SOFC technology.", "Experimental Section Experimental details are included in the Supporting Information.", "Conflict of Interest The authors declare no conflict of interest.", "Supporting information Supplementary Click here for additional data file." ]

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[ "Electrospun Ceramic Nanofiber Mats Today: Synthesis, Properties, and Applications Electrospun Ceramic Nanofiber Mats Today: Synthesis, Properties, and Applications EsfahaniHamid1* https://orcid.org/0000-0003-4540-321XJoseRajan2RamakrishnaSeeram3 1Department of Materials Engineering, Bu-Ali Sina University, Hamedan 65178-38695, Iran 2Faculty of Industrial Sciences & Technology, Universiti Malaysia Pahang, Lebuhraya Tun Razak, Gambang 26300, Kuantan, Malaysia; rjose@ump.edu.my 3Center for Nanofibers and Nanotechnology, Department of Mechanical Engineering, Faculty of Engineering, 2 Engineering Drive 3, National University of Singapore, Singapore 117576, Singapore; seeram@nus.edu.sg *Correspondence: h.esfahani@basu.ac.ir; Tel.", "/Fax: +98-81-3838-1601-10 1238 Ceramic nanofibers (NFs) have recently been developed for advanced applications due to their unique properties.", "In this article, we review developments in electrospun ceramic NFs with regard to their fabrication process, properties, and applications.", "We find that surface activity of electrospun ceramic NFs is improved by post pyrolysis, hydrothermal, and carbothermal processes.", "Also, when combined with another surface modification methods, electrospun ceramic NFs result in the advancement of properties and widening of the application domains.", "With the decrease in diameter and length of a fiber, many properties of fibrous materials are modified; characteristics of such ceramic NFs are different from their wide and long (bulk) counterparts.", "In this article, electrospun ceramic NFs are reviewed with an emphasis on their applications as catalysts, membranes, sensors, biomaterials, fuel cells, batteries, supercapacitors, energy harvesting systems, electric and magnetic parts, conductive wires, and wearable electronic textiles.", "Furthermore, properties of ceramic nanofibers, which enable the above applications, and techniques to characterize them are briefly outlined. electrospinning nano fabrication nano ceramic fibers materials characterization properties of ceramic materials 1.", "Introduction Ceramics are widely used in many applications due to their chemical and thermal stability, and high mechanical and electrical properties arising as a result of ionic and covalent bonds between the atoms composing them [1,2].", "Recently, ceramic fibers have been developed for many advanced materials industries due to the unique properties known only in ceramic materials—superior high oxidation and corrosion resistance, semiconducting, sensibility, electric charge storage, catalytic behavior, magnetic properties, reconstruction of crystal units, tailored phase transformation, surface modification and wide range of bio-compatibility, to mention just a few [3,4,5].", "The development of nanotechnology leads to advances in materials and creates innovative solutions to the drawbacks related to the bulk materials.", "With the decrease in the diameter of fibers that is required to make nanofibers, the physiochemical and structural properties of materials are modified according to the corresponding bulk materials.", "Several methods have been developed to fabricate NFs, such as template method [6], self-assembly [7], phase separation [8], melt blowing [9], drawing [10] and electrospinning method [11].", "Among them, electrospinning is a straightforward, cost-effective, and versatile technique that essentially employs a simple and economical setup to produce NFs in a variety of shapes and sizes.", "For example, typical electrospinning set ups for production of random (non-woven) and aligned (oriented) NFs are shown in Figure 1.", "In this method, a polymer solution or melt is charged by an electric force and deformed into a cone called a Taylor cone, when electrostatic force overcomes the surface tension and viscosity of a polymer droplet.", "The high voltage between the needle tip with an aluminum collector causes the jet to stretch into a finer filament with evaporation of solvents.", "Filaments are eventually deposited on a plate or rotary collator to produce randomly non-woven or oriented NFs, respectively.", "They are synonymously called fibrous mat, membrane or scaffold (see Figure 1).", "Electrospinning has been regarded as the most promising approach to produce continuous NFs and the fiber diameter can be adjusted from micrometers to nanometers [4].", "Electrospinning is a beneficial method to synthesize NFs of single and composite phases.", "Moreover, electrospinning has been applied to natural and synthetic polymers, carbons and ceramics.", "Fibers with complex architectures, such as ribbon-shaped, porous, core-shell, or hollow can be produced by electrospinning methods.", "It is also possible to produce nanofibrous membranes with designed aggregate structure including alignment, patterning, and two and three-dimensional nanonets [12].", "In recent years, considerable efforts have been undertaken for fabrication of ceramic NFs via electrospinning methods.", "Electrospun ceramic NFs are a specific classification of materials due to the morphology, microstructure, composition and properties which enable them to be used in diverse applications such as life science and health-care sectors, energy and environmental ones, agriculture and food, electronic and magnetic devices [13].", "Electrospun ceramic NFs have shown many unique characteristics and have enormous application potential in widely diverse areas.", "Considerable researches have been conducted on exploring the properties and applications of electrospun ceramic NFs.", "For example, flexible electrospun TiO2-SiO2 mats are capable to curve to 1.3–3.4 mm radius of curvature even after heat treatment, while bulk ceramics are known to be brittle [14].", "In another research, it is demonstrated that composite laminate electrospun mats increase the delamination strength, a great idea for using electrospun mats in industrial bonding [15].", "Hybrid ceramic/polymer fibers can be easily synthesized by electrospinning method.", "Advantages of electrospinning methods aid to fabricate composite NFs in which the ceramic nanoparticles (NPs), hydroxyapatite (HA) here, is randomly decorated on the PA6 fibers without agglomeration (see Figure 2) [16].", "This review focuses on the recent progress in electrospun ceramic NFs.", "Type of ceramic NFs, synthetic procedures, effective parameters to obtain ceramic NFs, surface modification and their applications are discussed with regard to the experimental findings.", "This review also covers special methods developed to characterize the mechanical, physical and electrical properties of electrospun ceramic NFs. 2.", "Types of Electrospun Ceramic Fibers As ceramic precursor solution does not have enough viscosity to make a jet during electrospinning, several successful methods have been developed to overcome this problem.", "Using a polymer reagent in spinning solution is the most successful method.", "Further, methods such as sol-gel route [17,18], which includes a polymerization stage, is an alternative for polymer reagents in the production of ceramic NFs via electrospinning.", "Ceramic elements are added to a polymer solution as ceramic NPs or as ceramic precursors.", "Viscose polymer solution that has the potential to combine one or more ceramic elements in one solution eventually results in production of single phase or composite ceramic NFs.", "In spite of kind of ceramic elements in solution, two scenarios can be assumed for collected NFs in mats after electrospinning (see Figure 3); (a) Single phase ceramic NFs are obtained by elimination of polymer reagent via a certain heat treatment procedure, (b) Ceramic/polymer hybrid NFs are synthesized without any more heat treatment.", "Ceramic NPs inside the electrospun NFs will be sintered together like fibers shape or be decorated on polymer NFs following first and second scenarios, respectively.", "It is worth mentioning that not only ceramic NPs are used inside the polymer NFs but also metallic NPs are assigned inside the polymer NFs for desired applications.", "For example, Pt, Cu and Sn NPs are added in the fabrication of PVP/metal NFs for direct ethanol protonic ceramic fuel cell application [19], or for micro surface-mounted components [20].", "Similar to the ceramic NFs fabrication procedure, metal NFs can be obtained by heat treatment but at lower temperatures.", "Pt, Sn, and Cu, metal NFs are obtained by calcination of as-spun fibrous mats at 300–450 °C after evaporation of polymer reagents [19,20] (See Figure 4).", "It is worth mentioning that amorphous to highly crystalized ceramic NFs can be obtained according to the heat treatment procedure.", "In following sections recent developments on monolithic (single phase) and composite (hybrid) ceramic NFs are reviewed. 2.1.", "Single Phase Ceramic Fibers Many ceramic fibers have been so far prepared by electrospinning method.", "Not only simple oxide ceramic fibers such as TiO2, Al2O3 and ZnO, but also complex oxide ceramic fibers such as CaCu3Ti4O12 and Li1.6Al0.6MnO4 have been synthesized by electrospinning.", "In addition, non-oxide ceramic fibers such as ZrC and Cu2ZnSnS4 are also synthesized via electrospinning method.", "Table 1 lists several recent simple and complex oxide and non-oxide ceramic NFs produced by electrospinning.", "Ceramic precursor is often used in the form of acetate, nitrate and carbonate, using the single phase and composite ceramic NFs that could be synthesized via processing appropriate solutions.", "Doping of a cation inside the crystal lattice of ceramic (e.g., Mg2+ into hexagonal ZnO) is another advantage of this solution based route.", "Deionized water, ethanol, methanol or their combination are applied for solving the ceramic precursor(s).", "Polyvinylpyrrolidone (PVP), polyvinylacetate (PVA), etc. are common polymer reagents that dissolves in many basic or acidic solvents.", "Dimethylformamide (DMF) and chloroform (CF) are sometimes added to polymer solution for better charge polarization.", "Stirring is carried out until a homogenous and clear solution obtained.", "This stage could be done in short period of 1 h or prolonged to 24 h.", "Adjustment of pH has significant role in dissolving ceramic and polymer precursors.", "As mentioned above, polymer concentration controls the viscosity of solution.", "Extra amounts of polymer not only result in thicker fibers but also causes the destruction of ceramic fibers and elimination of polymer during calcination.", "Heat treatment called calcination is preformed based on the nature of ceramic, for example, ZnO NFs are synthesized by calcination at 500 °C for 2 h [21].", "Calcination conditions and their effects based on the real experience are discussed in a separate Section 3.3.", "As can be seen in Table 1, the final morphology of ceramic NFs could differ based on the choice of polymers, spinning and calcination conditions, such as straight, smooth, tubular, hollow, shorten fiber, sintered particles and irregular shapes. 2.2.", "Composite Ceramic/Polymer Fibers The ceramic/polymer electrospun composite NFs exhibit high surface-to-volume ratios with unique structure controlled morphologies.", "The inherent properties of these nanostructured fibrous materials make them suitable candidates for various advanced applications.", "For example, polymer/silicate NFs are used in diverse applications from biomedical, carbon fiber fabrication, food packing, to sensing [82].", "Promising approaches to constructing biodegradable polymers and bioactive ceramics have been implemented via electrospinning of hybrid scaffolds [83].", "A list of recent products of hybrid electrospun NFs composed by polymer matrix and ceramic NPs and their applications are given in Table 2. 3.", "Fabrication of Electrospun Ceramic Mats 3.1.", "Assistant of Polymer Since ceramic precursor solution does not have enough viscosity to make a jet during electrospinning procedure, a polymer reagent is often used in spinning solution aimed at developing ceramic NFs.", "Mohammadi et al. [97] and Zadeh et al. [49] explained the role of polymer reagent in viscosity of the spinning solution of CaCu3Ti4O12 and mullite, respectively.", "Continuous electrospinning is carried out when the viscosity of electrospinning solution is optimized.", "Higher polymer content tends to increase the viscosity of the solution, eventually resulting in flat ribbon shaped ceramic fibers.", "Another role of polymer solution is to obtain fibers with different diameter and crystallinity.", "For example, a different mass ratio of zinc acetate/PVA (1:3, 2:3 and 1:1) causes increasing fiber diameter and crystallite size of ZnO [98].", "Similar results have been obtained for NiO NFs [52,99].", "Figure 5 presents how the diameter and the crystallinity of NiO NFs increase with increasing the ratio of nickel acetate/PVA in precursor.", "According to Table 1, PVP and PVA are the most commonly employed polymer to synthesize ceramic single phase NFs.", "This is because they have high solubility in a variety of solvents and good compatibility with many metal alkoxides.", "To produce ceramic fibers, first soluble salts of metal are dissolved in water or ethanol and then added to polymeric solution.", "Polymeric solution is often prepared by adding DMF and CF in order to adjust the resultant fiber diameter and to prevent bead forming [57].", "Co-solutions consist of optimized ratio of ceramic precursor with polymer reagent are mixed and then electrospun.", "After drying, calcination is the main step to produce ceramic single phase NFs.", "Recent findings indicate that mixing of PVP with PVA help to achieve ultrathin NFs.", "Saleemi et al. [100] synthesized magnesium cobaltite NFs using PVP, PVA and PVP/PVA (3:1) and observed that the average diameter of NFs decreased from 250 to 200 nm in the case of combined polymers.", "Average diameter is also decreased by using other polymer reagents such as polyethylene oxide (PEO).", "Starbova et al. [101] examined PEO in the fabrication of electrospun ZnO NFs and found more efficient viscous–elastic behavior of the high molar mass PEO under electro-hydrodynamic conditions compared to that of PVA.", "Finally, it is worth mentioning that there are many attempts to eliminate polymer reagents by using the sol-gel method.", "Chen et al. [17] produced mullite NFs in the absence of polymers.", "Essential viscosity required for electrospinning is achieved via controlling the hydrolysis step of sol gel. 3.2.", "Electrospinning Parameters and Procedures There are many parameters that affect electrospun ceramic NFs morphology.", "Among them, the amount and composition of polymer in the solution are the most significant factors, as explained by many researchers [85].", "However, operating device parameters also play a significant role in achieving different morphology and crystallinity of ceramic NFs.", "For example, shape and type of collector affect the morphology of electrospun NFs.", "For example, a range of needle to collector distances can be produced using a sloped collector for making multi-size fibrous mats [85].", "Physical and electrical properties, adhesion and density of the NFs on substrate are also depend on the type of collector geometry.", "Lamastra et al. [102] examined four kinds of collectors for measuring the transmittance of NiO electrospun NFs: Al collector, sputtered Ni on quartz, and bare quartz substrate.", "They found that Ni-quartz target resulted in higher density of NiO NFs, while NiO-quartz target depicted more adhesion with NiO NFs.", "Furthermore, humidity as another aspect of environmental parameters also effect on NFs morphologies and crystallinity.", "Tikekar et al. [67] studied the effect of humidity (RH ~25–60%) on the microstructure of TiO2 electrospun NFs.", "They applied a heated target to form NFs at higher humidity (>60%), and observed that at higher humidity excessive plasticization of the PVP is induced and individual nanocrystals of TiO2 are formed.", "There has been much interest in fabricating aligned NFs via electrospinning.", "Several methods are developed for arraying NFs in the same direction: collection of fibers across two parallel closely spaced substrates and collection of fibers by high speed rotating mandrel [103,104] are most common.", "Laudenslager et al. [103] reported that the parallel rotary disk (PDR) method has more advantages than the other method for aligned fiber production, besides it is the only method for fabrication of continuous NFs in diameter range of 100 to 1000 nm.", "Another interest in electrospinning is to fabricate twisted rope NFs.", "Since the NFs rope offers improved mechanical properties, these types have the potential to be used in many applications, such as artificial muscle and electronic devices.", "In this procedure, a tube is rotated with a motor and another is fixed to an iron support.", "Zheng et al. [90] successfully synthesized PVDF/CNT composite NFs rope for use in strain sensors.", "Synthesis of ceramic porous hollow NFs (e.g., Al2O3) is another interest in modified electrospinning devices.", "In this type of electrospinning device, an electrode is inserted into the PVC pipe to induce an electric charge into the solution and solution is loaded into the reservoir from which the solution flowed the pipe.", "The flow rate is determined by the difference of the air pressure between bottom of reservoir and inserted electrode pipe.", "Multiple pendent drops are formed at the holes in the pipe through changing the applied voltage and shape of the Taylor cones from which the polymeric jets are launched toward the grounded collector [105]. 3.3.", "Calcination and Heat Treatment Heat treatment of ceramic/polymer mats via electrospinning procedure has a critical role in the production of ceramic NFs.", "Heat treatment known as calcination, is carried out in accordance with the nature of ceramic and polymeric solution at different temperatures and soaking times.", "Table 1 provides a set of calcination conditions of many kinds of ceramic NFs recently fabricated.", "Calcination is often carried out in O2 atmosphere with regard to oxide ceramic fibers.", "However, other gases such as H2, N2 and Ar are purged into furnace to obtain non-oxide ceramic NFs.", "The effects of atmosphere on composition of electrospun Cu doped ZnO NFs have been investigated in two ways: first, the dried fibers are calcined at 450 °C for 3 h under flow of O2 and second samples calcined at 300 °C for 2.5 h in H2.", "The first procedure caused the formation of CuO, Cu2O, and ZnO, and the second procedure tended to in-situ reduction of CuO and Cu2O into Cu nanocrystals (NCs) [77].", "Not only calcination is preformed to eliminate the polymer part but it is also applied to change the crystallinity of ceramic NFs.", "For example, ZrO2 have gained much attention due to their use as catalysts, thermal barrier coatings and biomaterials regarding its crystal systems.", "Singh et al. [79] synthesized ZrO2 NFs by electrospinning method and they found that calcination at different temperatures resulted in tetragonal to monoclinic phases without disrupting the fiber morphology.", "The heat treatment parameter plays significant role in the final size and morphology of fibers.", "A low heating rate is often applied to ensure the removal of organic components without destroying the NFs appearance and also to avoid ceramic NFs breaking to small parts due to rather poor thermal shock resistance of ceramics [106].", "Gibbons et al. [41] examined calcination of (Pd/Cu) doped CeO2 in PVP matrix NFs via rapid (2 K·min−1) and slow (0.1 K·min−1) heating rate.", "A non-woven mat of CeO2 based NFs with average diameter <200 nm was achieved with slow oxidative calcination.", "However, with rapid heating, thicker fibers and micro-defects remained in the final mat due to melting and removal of polymer (see Figure 6).", "It is worth knowing that fiber structure is not always achieved by calcination.", "Our findings based on the literature review as shown in Figure 7 confirm the above statement.", "Smooth, straight, broken, short fiber, sintered fibers and particles, belt and ribbon, hollow and porous fibers could be the final morphologies after calcination of ceramic/polymer electrospun mats.", "The morphology of pristine fibers changes dramatically at different temperature of calcination depending on the polymer matrix and ceramic precursor.", "STA analysis of as-spun mats is usually employed to determine the optimum calcination temperature.", "Degradation of polymer reagent, ethanol, nitrates, carbonates and acetate groups in most as-spun mats are occurred at temperature <500 °C.", "A region can be observed at higher temperature in the differential scanning calorimetry-thermogravimetry (DSC-TG) curves such that no weight loss occurred after a certain temperature [31].", "The final stage of calcination is performed at this temperature to form single phase ceramic fibers.", "Figure 8 shows the SEM images of CaCu3Ti4O12 composite NFs calcined at different temperatures (600 to 1130 °C) [30].", "It is obvious that the morphology of the final NFs depends on the calcination temperature.", "Calcination at lower temperatures tends to form smooth surface NFs while higher temperatures tend to form porous ceramic NFs due to degradation of organic compounds (such as nitrates, acetates and PVP).", "However, further increasing of calcination temperature causes eliminating pores from surface of NFs, and suggests that coarse grained ceramics NFs are formed due to the sintering.", "Further heat treatment causes to NFs become a bulk ceramic.", "Achievement of morphology different form original electrospun fibers has been observed by several researches.", "For example, flower-like Li1.2Ni0.17Co0.17Mn0.5O2 microstructures was the favorable morphology to facilitate the diffusion of lithium ions into pores of fabricated mat as an electrode of a battery [107].", "Figure 9 shows how PVA/ Li1.2Ni0.17Co0.17Mn0.5O2 pristine NFs change to nanoplates (NPLs) with an open porous structure after calcination and finally transform to flower-like microstructure at elevated temperatures. 3.4.", "Surface Modification of Electrospun Ceramic Mats Two dimensional electrospun mats have high surface area in comparison to the other forms of materials.", "There are many attempts to enhance the surface activity of NFs.", "Pyrolysis, hydrothermal, carbothermal and other process have been performed on electrospun ceramic NFs to enhance their surface activity promoting biomedical, electronic, sensor applications.", "Pyrolysis of electrospun NFs is a new and effective method to beneficially allow for large scale NF production.", "In this method, only the pyrolysis step required to transform the polymers to ceramics at lower temperatures.", "This method is faster than common electrospun ceramic NF processing which has multistep production and needs elevated temperature [108].", "By pyrolysis of electrospun NFs at lower temperature not only oxide ceramic NFs can be produced but also non-oxide ceramic NFs (e.g., SiC, Si3N4, TiC) can be synthesized.", "SiO2, Si3N4 and Si2N2O nanowires (NWs) are achieved from electrospinning mats afterwards by pyrolysis under N2 flow at 1300 °C for 2 h.", "TiC NFs are also synthesized first by electrospinning of polyacrylonitrile and titanium isopropoxide solution and then thermally stabilized at 270 °C in air for 3 h and then carbonized and pyrolyzed under Ar at 1000 °C for 3 h [109].", "The hierarchical structure including fibers decorated with SiO2, Si3N4 and Si2N2O NWs possess a higher specific surface than simple NFs, which is more beneficial in gas sensor devices [110].", "Although microstructure NFs can be exchanged to desirable shape via pyrolysis method, there are some problems to obtain perfect NFs.", "Eick et al. [108] overcame breaking the fibers during pyrolysis by means of UV irradiation on mats that crosslinks the polymer and prevents fibers to flow during pyrolysis.", "The hydrothermal process is an effective method to improve surface activity of electrospun ceramic NFs.", "Figure 10 shows the effect of the hydrothermal process on ZnO NFs at 160 °C in aqueous medium containing hydrolyzed zinc acetylacetonate at different conditions [111].", "Time of hydrothermal processing affects the recrystallization and morphology of ZnO NFs.", "This is because of the adsorption of zinc hydrolytical products as well as an acetylacetonate group on selected crystal planes.", "Carbothermal reduction is employed to achieve hollow fibers.", "Generally, carbothermal reduction is carried out in two steps: the first step at lower temperature in vacuum and the second step at elevated temperature in N2 atmosphere.", "AlN and ZrN hollow NFs are synthesized by electrospinning of common precursor following carbothermal reduction.", "By this method, rough and hexagonal crystal of AlN and ZrN are formed on the surface of NFs.", "The outer diameter and thickness of hollow fibers are 500 and 100 nm, respectively [112,113].", "Surface modification of ceramic NFs has been achieved chemically using organic and inorganic solutions.", "In this case, ceramic or polymer/ceramic hybrid NFs are treated using an appropriate sol and subjected to controlled calcination in accordance with the nature of the secondary phase.", "Branched NFs of TiO2 NFs are achieved via immersing in V2O5 sol and subsequent calcination at 550 °C for 2 h at N2 atmosphere (see Figure 11) [66].", "Qin et al. [114] found that soaking ceramic NFs in water or air before or after calcination is also useful to change their microstructure.", "Functionalization is a practical method for synthesizing hollow NFs.", "Huang et al. [115] functionalized the SiO2 electrospun NFs and found that silica shell is covalently decorated on the hybrid fiber surface by hydrolysis and condensation of silyl functional groups with the tetraethoxyorthosilane (TEOS) in an ethanolic ammonia suspension.", "After thermal decomposition of the polymeric fiber templates, inorganic silica hollow fibers are formed that mimic the structure and morphology of the fiber templates.", "Plasma etching, sputtering and annealing of electrospun NFs can make the high surface area for electrospun NFs.", "SEM micrographs of SnO2 NFs modified by plasma etching and sputtering process at different conditions to achieve hierarchical NFs are presented in Figure 12 [116]. 4.", "Characterization of Ceramic Electrospun Mats The properties of electrospun NFs can be studied throughout different techniques.", "Microstructural features, mechanical, physical and electrical properties of ceramic NFs are different from those of bulk materials.", "Hence, the characterizations of electrospun NFs are discussed below. 4.1.", "Microstructure Electrospun NFs can either be randomly oriented in the length and width directions or in contrast be aligned unidirectionally in the plane of the mat.", "Directionality (angle distribution) of fibers histogram can be useful for studying the arrangement of fibers.", "For this matter, the number of fibers in each orientation is measured and then frequency versus angle is plotted in a graph.", "A typical angle distribution of SiOC fibers produced from different precursors is presented in Figure 13 [57].", "It is worth explaining that flat histograms represent the random oriented NFs, and histograms with a narrow and sharp peak present a preferred orientation.", "Furthermore, two peaks histograms demonstrate cross linked oriented fibers.", "Therefore, histograms shown in Figure 13 indicate both kinds of fibers have a preferred orientation. 4.2.", "Mechanical Properties The tensile strength of fibrous electrospun mats are measured using an electro-force planar biaxial test bench instrument via applying uniaxial stress in accordance to ISO 527-3 standard.", "Stretching rate and shape of the test sample are two critical factors to achieve accurate results.", "According to the displacement of fixture and loading force, a stress-strain curve is plotted to study the mechanical properties of mats such as elastic and plastic stage, Young module as well as ultimate tensile strength (UTS).", "The strain–stress curves of the PA66, PA66/MWCNT (multiwalled carbon nanotube) and PA66/TMWCNT (treated multiwalled carbon nanotube) are shown in Figure 14.", "As can be seen, MWCNT-based polymer composites have better mechanical properties than pristine polymers owing to the reinforcing effect of MWCNT.", "Mixing of CNT and MWCNT into polymer NFs causes a significant enhancement of mechanical properties due to enhancement of β phase and elasticity, and also formation of a stable three-dimensional conducting network [117,118].", "Xiang et al. [119] have also investigated the incorporation of CNT NFs inside the electrospun PA6 fibrous mats, and found that fiber-fiber load sharing can be enhanced by using each following methods; increasing friction between fibers, thermal bonding, and solvent bonding.", "Moreover, adding the NPs into polymer NFs usually has similar results.", "Al2O3 and TiO2 NPs as typical ceramic NPs modify the roughness of the fibers and affect the interfacial adhesion between the filler and the polymer matrix.", "Although Young’s modulus and tensile strength were improved with addition of NPs, a less pronounced effect was found for ductility and stiffness of electrospun mats [120,121].", "It is worth mentioning that using metallic cations (e.g., Fe3+) inside the polymer solution reinforces the fibers due to changing the pH, functionalization and enhancement of organic group attachments [122].", "Eventually it is worth mentioning that in some applications such as water filtration and tissue engineering, tensile strength is measured via two type methods; dry and wet conditions [123].", "The wet condition is carried out in the same way as the dry but firstly samples are immersed in a water or a bio-solution container for a certain period of time, and then pulled out and quickly examined by the above procedure. 4.3.", "Physical Properties 4.3.1.", "Porosity The total porosity of electrospun fibrous mats can be measured with different methods.", "Bulk density method, mercury intrusion porosimetry (MIP), X-ray computed tomography (X-CT), and Barrett-Joyner-Halenda (BJH) analysis are practical methods for determination of pore size and pore size distribution of electrospun ceramics mats.", "(a) Bulk Density Method The total porosity is calculated based on the following equation; (1) P o r o s i t y ( % ) = 100 − ρ 0 ρ where ρ and ρ0 are bulk and true density, respectively.", "Bulk density is calculated by dividing the weight by the volume of mat, and true density is measured by gas pycnometry method [57].", "(b) Mercury Intrusion Porosimetry (MIP) In this method, the pore size is measured in accordance with the external pressure needed to force the liquid into a pore against the opposing force of the surface tension of the liquid [57].", "The basic formula used in this method is: (2) P o r o s i t y ( % ) = V P o r e V P o r e + V A p p a r e n t × 100 where, VPore is the total pore volume of the test sample, and VApparent is the apparent volume of the test sample.", "For this technique, a porosimeter device is used for the analysis of pore structure of fibrous mats.", "(c) X-ray Computed Tomography (X-CT) This method is a NDT technique for preparing digital data of samples like those in electrospun fibrous mats by using computer processed X-ray to produce slices of specific areas of the body.", "Then a three-dimensional image is built by stacking a large series of axial slice and carried out for calculating solid fraction (SF).", "The porosity is then calculated via the following equation [124]; (3) P o r o s i t y ( % ) = 100 % − S F % (d) Barrett-Joyner-Halenda (BJH) BJH analysis is an analytical method to measure the pore size distribution of mesoporous materials.", "Electrospun ceramic mats (e.g., Zn2SnO4) can be easily characterized by this method [125].", "In this method, the amount of gas, preferably nitrogen, desorbed on the sample as a function of the partial gas pressure is measured at 77 K.", "The modified Kelvin Equation (4) is then used to relate the amount of adsorbate removed from the pores of the material, as the relative pressure (P/P0) is decreased from unity to a lower value, to the size of the pores [126]. (4) r k = − 2 γ V R T L n ( P / P 0 ) where rk is Kelvin radius; V the mole volume of nitrogen; and γ the surface tension of liquid nitrogen. 4.3.2.", "Gas Permeability Gas permeability of electrospun fibrous mats are measured under inert gas flow (e.g., N2 or Ar) on a disk with a certain diameter, mostly ~35 mm.", "A device calculates the permeability constant and uses Forchheimer’s equation as follows [57]; (5) P a 2 − P b 2 2 P b L = μ k ν s where Pa and Pb are the absolute gas pressures at the entrance and exit of the sample, respectively. vs and L are the superficial fluid velocity and sample thickness, respectively.", "F and μ are gas density and viscosity, respectively. 4.3.3.", "Water Permeability The water permeability test is performed using a dead-end filtration cell with a certain thickness of membrane and filtration area.", "Before water permeability test, usually membranes are immersed in ethanol for 1 h, and then, the membranes are sufficiently washed with de-ionized water.", "The deionized water is filled in a reservoir and the filtration pressure is maintained by N2 or Ar gas.", "The weight of the permeated water is measured for a certain period of time and applying pressure, and the water permeability is calculated by Equation (6) [127]: (6) Water permeabilty = m tAP where m is the mass of the permeated water (kg), t is the sampling time (s), A is the effective membrane area (m2), and P is the pressure (bar). 4.3.4.", "Turbidity The turbidity test is performed to observe the rejection of particulates and changes in the turbidity.", "The certain amount of target solution is prepared and the test is performed using a dead-end filtration system at room temperature as well as at certain pressure.", "According to the turbidity of the samples, rejection rate is calculated using the following equation: (7) Rejection rate ( % ) = ( 1 − C f C i ) × 100 where Ci is the initial and Cf is the concentration of permeate.", "Ci and Cf can be calculated by UV-Vis technique or using a turbidimeter [127]. 4.3.5.", "Thermal Conductivity Thermal conductivity has an important role during calcination of ceramic NFs.", "Fast weight loss of polymeric compound creates more pores which are reasons for decreased thermal conductivity.", "Phonon scattering centers and the phonon thermal conductivity depend on the concentration of defects.", "By decreasing the grain size of the polycrystalline sample, the defects increase which provide effective phonon scattering centers and thus reduce the phonon thermal conductivity.", "In addition, the presence of porosity also has large effects in decreasing the thermal conductivity of a solid [46].", "The thermal conductivity of a polycrystalline ceramic NFs (e.g., La2Zr2O7) can be calculated by the following equation [128].", "This equation is valid for temperatures lower than 800 °C. (8) κ = C v ν m Λ / 3 where Cv is the specific heat, νm is the speed of sound and Ʌ is the phonon mean-free path. 4.3.6.", "Gas Sensing Gas sensing test is carried out generally by mounting the interdigitated electrodes (IDEs) in a quartz tube placed inside furnace.", "The IDEs are connected to a resistance monitoring setup via platinum wires.", "The cyclic exposure of the sensors to the analyte gases (e.g., H2 and NH3) is achieved with the aid of mass flow controllers.", "The total gas flow rate is maintained constant during the sensing test, which is carried out at a desired temperature.", "For ensuring stable resistance, the sensor is equilibrated in dry air overnight at the required temperature before beginning of the gas sensing experiments.", "During equilibration, dry air is flowed at a constant rate (e.g., 200 cm3/min) and sensor signal, which represents the magnitude of the change in electrical resistance when exposed to analyte gas, is defined using the following equation [99]; (9) d R R = R g a s − R a i r R a i r where Rgas and Rair represent the measured resistances when the sensors are exposed to the analyte gas and air, respectively. 4.3.7.", "Hydrophobicity To investigate the hydrophilic or hydrophobic properties of electrospun mats, contact angle of a liquid on its surface is measured.", "For this technique, water, ethanol or their mixture is used to measure the contact angle.", "It is worth knowing that the surface tension of the mixture solution decreases with adding the ethanol to water.", "The height (y) and the half width (x) of the formed droplet on the target surface are measured to calculate the contact angle (θ) using the following equation [129]: (10) cos θ = x 2 − y 2 x 2 + y 2 It is worth mentioning that the electrospun fiber mats are capable to be superhydrophobic, hydrophobic and hydrophilic.", "There are some critical parameters affecting the water contact angle (WCA) values: porosity, pore size, pore size distribution and surface roughness that depend on morphology of electrospun fibers.", "Pore size and surface roughness also depend on fiber diameter.", "Cho et al. [129] showed that the porosity sharply increases as the fiber diameter increases and reaches a plateau after a critical fiber diameter.", "The fiber mats with a large deviation of fiber diameter and high surface roughness show a large change of the contact angle.", "Furthermore, single phase electrospun polymer NFs are superhydrophobic and hydrophobic.", "By adding the ceramic NPs to polymer NFs, WCA decreased and hydrophilic surface are formed with regard to the nature of molecular groups of ceramic (e.g., nitride, oxide, hydroxyl, phosphate) [130]. 4.3.8.", "Zeta Potential The zeta potential measurement of electrospun NFs mats are different from powder samples that require specimen holder preparation prior to use a commercial Zetasizer.", "For this technique, first two acrylic plates are machined and assembled to form a microfluidic channel (150 μm high, 2.0 mm wide, and 30 mm long).", "A frame is formed outside the hole where electrospun NFs are spun to cover around the frame (see Figure 15).", "Two electrodes for the measurement of streaming currents are housed in the top plate.", "A programmable micropump is used to apply fluid pressure with controlled flow rate (0.1 to 1.6 mL·min−1).", "Different pH buffer solutions can be used in this method in order to characterize the zeta potentials [131]. 4.4.", "Electrical Properties 4.4.1.", "Dielectric Constant There is no direct method to measure the dielectric constant of NFs because the dimensions of NFs are much smaller than those required for standard measurements.", "Another problem occurring during measurement of NFs is the existence of pores in the NFs mats.", "Researchers solved this problem by applying the mixture rule as shown in Equation (11) [30]. (11) log ε c = ν 1 × log ε 1 + ν 2 × log ε 2 where εc, ε1 and ε2 stand for the dielectric constant of a ceramic/polymer composite, polymer, and ceramic, respectively; ν1 and ν2 represent the volume fraction of the polymer and ceramic, respectively. 4.4.2.", "Electrolyte Uptake In order to measure electrolyte uptake and ionic conductivity of electrospun mats which are important in many applications, the mat is immersed in liquid electrolyte for a period of time.", "After immersion, the membrane is taken out of the electrolyte solution and the excess electrolyte solution on the surface of the separator is wiped off with filter paper.", "The uptake of electrolyte solution is determined using the following equation [86,132]; (12) U p t a k e ( % ) = W − W 0 W 0 × 100 where W0 and W are the weights of the electrospun mat before and after soaking in the liquid electrolyte, respectively. 4.4.3.", "Ionic Conductivity AC impedance measurements using an impedance analyzer over the variable frequency ranges and amplitude are performed to measure the ionic conductivity and interfacial resistance of nanofibrous mats [86].", "The following procedure is used to measure ionic conductivity of electrospun mats.", "First the electrolyte sample is sandwiched between two stainless steel electrodes and the impedance measurements are performed at certain amplitude over the desired frequency range.", "The cell is kept for some time (e.g., 5 h) to ensure thermal equilibration of the sample before measurement.", "The interfacial resistance Rf between the polymer electrolyte and lithium metal electrode is measured at room temperature by the impedance response of Li/polymer electrolyte/Li cells over the frequency range 10 mHz to 2 MHz at an amplitude of 20 mV.", "The electrochemical stability is determined by linear sweep voltammetry (LSV) of Li/polymer electrolyte/steel cells at a scan rate of 1 mV/s over the range of 2–5.5 V at 25 °C [132]. 4.4.4.", "Battery Efficiency The following procedure uses the battery test of electrospun mats.", "Two-electrode lithium prototype coin cells are fabricated by placing the electrospun polymer electrolyte between lithium metal anode and carbon coated lithium iron phosphate (LiFePO4) cathode.", "Then the electrochemical tests of the Li/polymer electrolyte/LiFePO4 cells are conducted in an automatic galvanostatic charge–discharge unit at 25 °C at a certain current density.", "The activation of electrospun membrane to prepare polymer electrolyte and the fabrication of test cells are carried out in an argon-filled glove box with a moisture level <10 ppm [132]. 4.4.5.", "Permittivity, Magnetic Permeability, and EMI Shielding Efficiency (SE) The ASTMD-4935 standard is used for measuring the permittivity, magnetic permeability, and electromagnetic interface (EMI) shielding efficiency (SE) of two-dimensional materials like electrospun mats.", "In this method, a network analyzer equipped with an amplifier and a scattering parameter (S-parameter) test set over a frequency range of 800–8500 MHz.", "The annular disk made of electrospun mats are prepared by punching machine, and EMI shielding efficiency is calculated using the S-parameters [88,133]. 4.4.6.", "Harvest Energy Performance In order to preform the bending test examination, first NFs are collected on an interdigitated electrode plates as shown in Figure 16a and then, in order to study the effect of larger deformations on the output voltage of the electroactive NFs, a finger which protected by an insulator glove in order to prevent interferences from human bioelectricity, is used to apply a periodic dynamic loading on the top of the generator by simple tapping during which, the positive and the negative output voltage is measured.", "According to the results obtained by Nunes-Pereira et al. [93] the highest output voltage depends on mechanical properties of NFs.", "Moreover, decoration of polymer NFs by ceramic NPs is not always appropriate for energy harvest application because of increases of mechanical strength. 5.", "Applications of Ceramic Electrospun Mats Ceramic NFs have recently been recognized as advanced materials due to their special properties and microstructures [12].", "In accordance with our knowledge, several applications can be assumed for ceramic NFs: catalyst, membrane, sensor, biomaterial, fuel cell, and parts of electronic device and batteries.", "Ceramic NFs application is not limited to the above-mentioned fields, new application areas have been introduced for using of NFs such as fire-resistant fabrics or sound adsorbent materials.", "Moreover, the microstructure, composition and size of NFs can be controlled via electrospinning procedure, thus high practical NFs are developed in accordance with requested applications. 5.1.", "Catalysts and Photocatalysts Ceramic NFs are widely used in many photocatalystic applications, and fortunately they can be fabricated in different morphology such as hollow, porous, belt and solid via electrospinning procedures.", "Photocatalytic activity of electrospun ceramic NFs are generally carried out by using different organic targets such as methylene blue (MB), methylene orange (MO), and Rhodamine B (RhB).", "Choi et al. [134] demonstrated a new type of visible light-induced photocatalyst, using fluorescein molecules, TiO2, and gold NPs decorated on electrospun polymer NFs.", "It was found that the photo degradation efficiency of TiO2/polymer microstructure is nearly three times greater for MB than Degussa P25, which was used as a control material.", "Zhao et al. found that the decomposition rate of MO by branched TiO2/V2O5 hybrid NFs increased by ~96% relative to single phase TiO2 NFs.", "It is because of formation of V4+ and Ti3+ on the surface of NFs which have narrow band gap and lower electron-hole recombination rates [66].", "In spite of the benefits of electrospun NFs, it is worth mentioning that photocatalytic activity of some ceramics (e.g., TiO2) prepared by hydrothermal reaction is higher than that prepared by blended spinning [135].", "In accordance with the results obtained by Dong et al. [136] ZnO nanobelts (NBs) show the best photocatalytic performance for the degradation of RhB.", "Furthermore, it is found that the deposition of Au NPs on ZnO NBs can further enhance the photocatalytic activity owing to the formation of ohmic contact.", "Pascariu et al. [137] also showed that the efficiency of electrospun ZnO NFs for degradation of RhB is improved by incorporation of SnO2 inside the fibers for an optimum Sn/Zn molar ratio of 0.030.", "In addition, there are many studies on the photocatalysis property of electrospun NFs on actual targets.", "Wang et al. examined the electrospun Ni/Al2O3 NFs as a catalyst on the dry reforming of methane.", "They studied the effect of calcination temperature on the catalyst performance and found that the catalyst reactivity in the dry reforming of methane decreased with increasing calcination temperature.", "Furthermore, more and uniform Ni NPs are produced in attachment on NFs at high reduction temperatures.", "The reduction temperature effect is also confirmed by the reactivity during the dry reforming of methane [54].", "In another work, Hassan et al. [32] explained that electrospun CdTiO3 NFs have the potential for the removal of pollutants and noxious wastes.", "They found that calcination of as-spun NFs has better results for photocatalytic activities due to higher crystallinity and a red shifted absorption wavelength.", "Not only are common ceramic NFs (e.g., TiO2, Al2O3 and ZnO) used in photocatalysis application, but advanced ceramics are also assigned for photo- and the other catalysis applications.", "For example, electrospun SiO2 doped Bi2MoO6 NFs degraded MB with a high photocatalytic rate under sunlight compared to pure Bi2MoO6.", "This enhancement is because of presence of defects on the surface of SiO2 and at the SiO2–Bi2MoO6 interface [59].", "In another work, electrospun BiFeO3 NFs were successfully used for removing of 97% RhB.", "The porous BiFeO3 membrane also exhibit ferromagnetic behavior at room temperature with coercively ~170 Oe, saturation magnetization ~4.4 emu/g and high efficient absorbent [27].", "Leindeckern et al. [51] evaluated optical properties of electrospun Nb2O5 NFs and found that the optical energy gap reduced to ~3.32 eV with increase in calcination temperature.", "Nb2O5 NFs has been suggested as a photocatalyst because it can be easily recovered and recycled.", "In another work, the catalytic property of La0.6Sr0.4Co0.2Fe0.8O3−δ (LSCF) NPs coated on electrospun yttria stabilized zirconia NFs was compared with the materials produced using the conventional powder method.", "It was found that the exchange current of cathode made from the NFs (145.06 mA·cm−2) is much higher than that of powders (81.82 mA·cm−2), this increment has been attributed to the increase of triple phase boundary by the fiber structure [80].", "Electrospun (Pd/Cu) doped CeO2 NFs has also been evaluated for the water gas shift (WGS) catalytic reactor used in fuel cell systems, coal gas processing, and other applications [41].", "More than 60 h testing of this NFs catalyst in the WGS environment (5% CO, 10% H2O, balance Ar) at 400 °C indicated high WGS activity.", "The electrospoun Lu2SiO5 NFs have been studied for photo-luminescent properties; and the role of Ce3+ in the fiber on the emission efficiency was investigated [48].", "These NFs have a strong emission peak located at ~403 nm corresponding to the transitions of Ce3+ 5d1→4f1.", "Findings indicated that 1% Ce has the stronger light emission.", "In another similar work, the photo-luminescent properties of electrospun Eu3+ doped Gd2O3 NFs has been studied.", "The main finding of that study was an increase of the luminescent intensity and fluorescence lifetimes of Eu3+ doped Gd2O3 NFs with increase in concentration of Eu3+ or increase size of NFs [138].", "Furthermore, study on the photocatalytic properties of Mo doped BiVO4 electrospun NFs demonstrates that doping Mo into BiVO4 enhance the photocatalytic activity and dark adsorption ability.", "Liu et al. [139] explained that a small amount of Mo doping into BiVO4 can efficiently separate the photo-generated carries and improve the electronic conductivity. 5.2.", "Filtration and Separation It is necessary to implement remediation techniques to remove the organic and inorganic pollutants from gas and liquid phase polluted environment because they are harmful for ecosystems and human health.", "The remarkable properties of electrospun membranes, i.e., surface area, high open porosity, and interconnected porous structure, mean that they are one of the utmost promising and versatile filter media for fine particle filtration and separation.", "Electrospun filter media based on different polymer systems such as PA6, PA66, PAN, PU, PVA, PEO, PC, silk, copolymers such as PAN/PMMA, PVC/PU, or strengthened by ceramic such as PA-6/boehmite and PAN/TiO2 are widely used in filtration media [140].", "In accordance with certain types of pollutions, appropriate single phase or composite ceramic electrospun NFs are used to remove organic and inorganic pollutants; and kinetics models have been developed for each type of pollutions.", "For example, Kim et al. [22] used electrospun γ and β phase of alumina NFs for adsorption of N2 gas and methyl orange form liquid.", "The isotherms of N2 gas adsorption by alumina NFs are in agreement with results obtained by mesoporous structure.", "It is found that the pseudo second order kinetic model fits better than first order in the adsorption of methyl orange.", "This means that NFs compose a two-dimensional mat which behaves like a surface.", "Removing heavy metals is an important topic of nano filtration field.", "Hota et al studied sorption of Cd+2 ions by electrospun PA6 and PCL membrane inclusion of ceramic boehmite NPs and found that sorption capacity of polymer/boehmite is much higher (0.2 mg/L) than polymer NFs alone (0.002 mg/L) [94].", "Another study demonstrated for electrospun PCL/clay and PVA/clay that NFs are suitable for use in heavy metal removal of cadmium (Cd+2), chromium (Cr+3), copper (Cu+2) and lead (Pb+2) from water due to the high surface activity [141].", "Further studies showed that the adsorptive property of fly ash and photocatalytic property of TiO2 can introduce different functionalities on PU mat for water purification.", "Kim et al. [142] studied the adsorption of heavy metals (Hg, Pb) and organic element (e.g., methylene blue) by PU decorated with fly ash and TiO2 NPs for water purification.", "They found that adsorption capacity is improved in comparison to pure PU NFs.", "Oil pollution problem has prompted a necessity to develop a cost-effective and environmentally-friendly way of oil spill cleanup.", "Recent studies by Jiang et al. [143] showed that electrospun magnetic composite NFs can help to remove oil pollutants from waste water.", "Jiang et al. indicated that the electrospun magnetic PVDF/Fe3O4 NFs can be potentially useful for the efficient removal of oil in water and recovery of sorbent material [143].", "In another similar work, the adsorption of organic pollutants has been investigated by magnetically separable TiO2-coated SrFe12O19 NFs.", "For this matter, first SrFe12O19 NFs were fabricated by electrospinning procedure and post-calcination, and then TiO2 was coated on the fiber surface by dipping those fibers in the tetrabutyl titanate solution.", "Li et al. [65] explained that SrFe12O19 NFs causes an improvement in the decolorizing efficiency of MB by TiO2 under UV–vis irradiation.", "Moreover, these fibers can be recollected easily with a magnet in a photocatalytic process and they effectively avoided the secondary pollution of treated water. 5.3.", "Biomedical By reviewing recent developments in electrospun multifunctional scaffolds, it is confirmed that the designing and fabricating the scaffolds showing multiple functions has gained preliminary importance.", "High open porous structure, compatible mechanical strength, biodegradability and biocompatibility of electrospun scaffolds promote them as optimal microenvironment for cell proliferation, migration, differentiation, and guidance for cellular in growth at host tissue.", "Moreover, electrospinning can produce nanofibrous scaffolds that are highly desirable for wound dressing, drug delivery, tissue engineering and other biomedical applications [140,144,145].", "Our investigations show that combination of biodegradable polymers with bioactive inorganic materials is necessary for biomedical application, and single phase biomaterials have limited utilization.", "Electrospinning method is capable to fabricate composite ceramic/polymer NFs which is requested for tissue engineering and other biomedical applications.", "The fibrous scaffold of HA/biopolymer could recently develop its potential in the field of tissue engineering and bone regeneration.", "Although electrospun membranes are famous for high surface area, which facilitates efficient adsorption of biomedical reagents, the incorporation of ceramic non-stoichiometric HA NPs inside the PA6 causes the sorption efficiency of protein BSA molecules to be improved 5 times more than one pristine PA6 NFs.", "By homogenous dispersion of HA NPs inside the PA6 NFs, highly porous materials (~77%) are achieved that result in sorption of 60 mg·cm−2 BSA molecules.", "The other benefit of ceramics elements using in biomedeical purification is their ability to change surface functionality and affinity; higher positive surface electric charge causes more adsorption of negative bio-molecules [127].", "Moreover, addition of HA NPs into NFs modifies hydrophobicity of electrospun NFs that adhere to more favorable human cells.", "For this matter, Suslu et al. studied electrospun HAp/PHBV mats, and they found that surfactants strongly activate the precipitation rate of the apatite-like particles and decrease the percentage crystallinity of the HAp/PHBV mats [89].", "Li et al. studied the dispersion of HA in PCL NFs and found that the tensile strength and Young’s modulus increased.", "Furthermore, composite NFs were examined for bioactivity and toxic in vitro tests.", "Findings showed that new HA formed on the HA sites and composite NFs were non-toxic to fibroblasts and osteoblasts [146].", "Combination of biomimetic nanofibrous scaffolds with bio-functionalized elements is a new strategy for promoting bone regeneration, especially in bone tissue engineering.", "Zhang et al. [147] fabricated a zein (a kind of protein) fibrous membrane incorporated with bone matrix-mimic ceramic HA NPs by electrospinning method.", "It is observed that the zein/HA membranes can support cell proliferation and shows promise in bone tissue engineering applications.", "Su et al. [148] studied the secretion levels of Collagen I and fibronectin on electrospun PLA NFs coated by calcium silicate.", "They found that using inorganic apatite coatings tend to make suitable conditions for bone tissue engineering.", "In another work, Liu et al. [149] investigated the effect of HA/chitosan seeded with bone marrow mesenchymal stem cells (BMSC) for bone regeneration.", "Their findings showed HA/chitosan/BMSC is useful for bone reconstruction and tissue engineering due to the activating of intergrin-BMP/Smad signaling pathway of BMSCs on mentioned scaffold.", "In another research, electrospun TiO2 NFs have been used in a multilayer system of TiO2 nanofiber/graphite oxide paste/glassy carbon electrode to voltammetric determination of levodopa (l-DOPA) in aqueous media [68].", "The mentioned that the electrode exhibited effective surface area, more reactive sites and excellent electrocatalytic activity due to assignment of TiO2 NFs.", "It can be mentioned that this method is capable of quantifying l-DOPA in human cerebrospinal fluid, blood serum and plasma.", "This is because of the good linear relationship with a limit of detection of 15.94 nM and good sensitivity of 0.0806 μAμM−1.", "Drug delivery from electrospun fibers is an active area of research because electrospun materials are metastable superhydrophobic and hydrophobic materials and their rate of wetting controls drug release from the surface of material [150].", "There are many articles published recently with regard to this application.", "Not only have meloxicam (MX) immobilized biodegradable chitosan/PVA/HA based electrospun NFs shown good biocompatibility, but were also confirmed to be non-cytotoxic and show very good proliferation of vero cells.", "It is suggested that this material may have effective utilization in periodontital treatments [151].", "There are many efforts for utilization of ceramic NPs and NFs for biomedical applications.", "The unique antimicrobial properties as well as protein release mechanisms of SiO2 make the electrospun polymer-silicate hybrid NFs a candidate for wound dressing applications [82].", "Suitable mechanical properties and positive magnesium release from PCL/MgO/Keratin NFs have been developed the composite materials with structural and material properties that will support biomedical applications and musculoskeletal tissue engineering [152].", "The potential use of the electrospun PLA/Al2O3 NFs for biomedical application was investigated by Kurtycz et al. [87].", "They found that the PLA/Al2O3 NFs mat is not toxic in indirect cytotoxicity evaluation with human skin fibroblasts.", "Furthermore, cell culture studies revealed that cells had normal shapes and are integrated well with surrounding NFs.", "In another research, Guo et al. [58] prepared Ag/SiOC composite NFs via electrospinning method and possessed antibacterial activity for both Gram-negative E. coli bacteria and Gram positive s. aureus bacteria.", "It was explained that Ag/SiOC composite NFs are a promising material for antibacterial filtration application.", "Eventually, electrospun PCL/CaO NFs containing biodegradable and ceramic particles are used for tissue engineering [153].", "Antibacterial activity results of the above-mentioned NFs show non activity, and MC3T3-E1 cell viability demonstrate the highest levels of activity for CaO-loaded matrices containing gelatin after 7 days in culture.", "Therefore, CaO NPs loaded electrospun mats could be a potential material for application in bone tissue engineering. 5.4.", "Fuel Cells Many recent researches have focused on new materials for intermediate temperature solid oxide fuel cells (SOFSc) due to long term stability of electrochemical activity and low energy consumption [55].", "Catalytic activities of the cathode materials in SOFCs depend on oxygen ionic conductivity and oxygen transport kinetics.", "Besides, the cathode performance is also closely related to the microstructures such as porosity, particle sizes and particle connectivity.", "Hence, Liu et al. [55] synthesized Pr0.4Sr0.6Co0.2Fe0.7Nb0.1O3−δ (PSCFN) NFs via electrospinning method to evaluate their usefulness as cathode in SOFCs.", "The PSCFN NFs was infiltrated by Gd0.2Ce0.8O1.9 (GDC) precursor to provide the composite cathode.", "It was found that the PSCFN–GDC (1:0.10) had excellent stability of electrochemical activity under a current density of 200 mA·cm−2 for 100 h at 800 °C.", "Their findings prove that the PSCFN–GDC composite NFs can act as a highly efficient cathode candidate for the intermediate temperature SOFCs.", "In another work, electrospun GdBaCo2O5+δ (GBCO) NFs calcined at 1000 °C were used as a cathode for electrochemical performance analyses.", "It is suggested that this procedure is time- and cost-saving and easy for manipulation as compared with the fabrication process using sol-gel method.", "Furthermore, the homogenous network structure of the GBCO cathode prepared with electrospinning route is believed to enhance the cathode electrochemical activities and realize improved performance.", "It is also suggested that it can serve as a promising cathode material for intermediate temperature SOFC [38].", "The performance of electrospun carbon NFs supported Pt catalyst as electrodes and hydrocarbon based sulfonated polyether ether ketone (SPEEK) as electrolyte in proton exchange membrane fuel cells have been investigated by Padmavathi et al. [154].", "They show that, compared to commercially available Pt/C catalyst and Nafion-117 membrane, the electrospun carbon /Pt NFs membrane showed higher power density (294.7 mW/cm2). 5.5.", "Sensors By reviewing the recent developments of electrospun ceramic NFs, it is recognized that these materials can construct a powerful platform to understand and design practical sensors.", "This is because of their high open porous structure and good mechanical strength.", "On the other hand, loading nano functionalized elements on the electrospun scaffolds promote sensing ability of these materials in biomedicine, waste water and gas treatment, air filtration and other utilizations.", "There are many studies about the potential application of electrospun NFs with regard to biosensors.", "Stafiniak et al. evaluated the electrospun ZnO NFs biosensor by a novel method based on the standard microelectronic device technology and using AlNx amorphous thin film [72].", "They found that the reversible response to physiologically relevant BSA concentrations in aqueous solution reached a high sensor current.", "In another work, the electrochemical response of LaMnO3 fibers modified carbon paste electrode (LaMnO3/CPE) for fructose determination has been evaluated in the 0.4–100 μM range and a low detection limit (0.063 μM) was found in comparison with other modified electrodes [44].", "Semiconducting SnO2, ZnO, TiO2, and CeO2 NFs are widely used as gas sensors due to changes in the number of electric charge carriers caused by reduction/oxidation reactions occurring at their surfaces [62].", "Therefore, attention to the surface area and surface activity are the key factors for ceramic NFs in gas sensing application.", "Recent research demonstrates the potential of ultra- sensitive gas detection at low operating temperature.", "Kim et al. [60] used SnO2 NFs as a gas sensing device for NO2 and CO gases by new synthesis method.", "In comparison to conventional micro scaled gas sensor devices, prototypes comprising of a random network of electrospun SnO2 NFs do not require higher operation temperatures.", "The detection limit of SnO2 NFs gas sensor device is 150 ppb NO2 at 185 °C.", "Furthermore, the chemical composition of NFs has a significant role in sensing of elements.", "Xu et al. found that not only is hydrogen sensing performance improved by doping Al into SnO2 NFs, but also response time (∼3 s) and recovery (less than 2 s) become rapid.", "It is believed that changing the crystals of SnO2 NFs by incorporation of Al is main reason for this phenomenon [61].", "Similar results have been observed by doping the Eu3+ cations into SnO2 enhancing significantly sensing ability of pure SnO2 NFs [63]. 2 mol % Eu doping to SnO2 causes increasing sensing two times higher than that of the pure SnO2 NF sensor at an operating temperature of 280 °C.", "In another work, SnO2–CeO2 composite NFs exhibited the highest response to ethanol.", "This is because catalytic activity of CeO2 is not formed in compositions of Ce content lower than 6 mol % [62].", "It is worth mentioning that, with the modification of the microstructure and fabrication process, high sensitive NFs can be achieved.", "Samanta et al. [155] explained that parallel electrospun ZnO NFs can be used for detection of lower concentration gasses (lower than 15 ppm) due to crystal structure and orientation of ZnO NFs.", "Among the different kinds of ZnO microstructure for sensing gases (e.g., acetone), Wei et al. [156] investigated the bristlegrass-like ZnO NFs for acetone sensing.", "They showed that electrospun products have fast response, good selectivity and repeatability in acetone sensing at 215 °C, which it is attributed to the bristlegrass nanostructure.", "In another work, Giancaterini et al. [69] reported a relative response of ~12.4 and 97% of full recovery using electrospun WO3 NFs which enabled NO2 sensing as low as 400 ppb.", "Another sensing aspect of electrospun NFs is to detect heavy metals, nitrate, carbonate and other elements in waste water or air that make online monitoring of pollutants in real environments.", "Electrospun G/PANI/PS hybrid NFs have been used in an electrochemical sensor to sense the Pb2+ and Cd2+ due to the high surface area and electrical conductivity [84].", "In this case, a linear range of 10–500 μg·L−1 was obtained for both Pb2+ and Cd2+; and limits of detection were found to be 3.30 and 4.43 μg·L−1 for Pb2+ and Cd2+, respectively.", "Hollow ZnO NFs have been investigated as an explosive nitro-compounds sensor and it was found that these NFs could successfully sense the nitro compounds; however, the sensing performance is greatly affected by the molecular structure of the nitro compounds [73].", "In another work, Pascariu et al. [157] suggest that NiO–SnO2 NFs can be used as active nanostructures for humidity sensors due to the electrical results obtained under humidity.", "They believe that the significant effective surface of NiO–SnO2 NFs is the main reason for increasing the conduction in the water environment.", "Furthermore, the porous electrospun Li+ doped SnO2 NFs also exhibited ultrafast response and recovery time within 1 s at a relative humidity level of 85%.", "Hence, the electrospinning method provides ultrafast sensors for practical applications, especially fast breathing sensors [158].", "By using the one dimensional electrospun core-shell TiO2-Al2O3 NFs online sensing to H2S, CH3OH and C2H5OH in N2 background is possible, but it should be mentioned that sensibility is not the same for all pollutants and the highest amount (three times more than the others) has been recorded for C2H5OH gas [159].", "Application of electrospun NFs are not included only to above items; however, new application can be assumed for these materials.", "Zheng et al. [90] could successfully synthesize twisted PVDF/CNT composite NFs via modified electrospinning procedure.", "In comparison, with aligned arrays, twisted PVDF/CNT composite fiber ropes showed enhancement in mechanical and electrical properties.", "By adding more CNT into PVDF NFs (16.7%) tensile strength improved 3.5 times and electric resistance decreased from about 6 to 2 MΩ.", "Therefore, microscale strain sensors application for electrospun PVDF/CNT composite products is assumed.", "We know that bulk ceramic based sensors are usually used for high temperature sensor applications.", "However, negative temperature coefficient like NiO can be used as thermally sensitive resistor element in low temperature range.", "The temperature sensor performance of the electrospun NiO NFs has been examined by George et al. [53] in 30–100 °C temperature range.", "A linear trend for electrospun NiO NFs was observed that makes this material suitable for thermistor applications. 5.6.", "Batteries Lithium ion batteries (LIBs) have attracted increasing attention due to their high energy density, long cycle life, lightweight and low environmental impact.", "Recent efforts have been focused on finding new electrode materials including new composition and attractive microstructures similar to the electrospun NFs.", "For example, mesoporous CNT/electrospun carbon NFs electrodes are applied as a binder-free electrochemical electrode for the LIB.", "The super high porosity mat presents many adsorption sites of lithium ions, and higher electrical conductivity [160].", "The electrospun carbon NFs interlayers induce the Li ions to form uniform Li metal deposits on the fiber surface and in the bulk to strengthen the cycling stability of the Li metal anodes [161].", "In the following, activities on electrospun SiO2, Al2O3 and SnO2 based NFs for LIB are reviewed.", "Electrospun silica (SiO2) fibers with average diameter of ~700 nm are added to a ternary poly (ethylene carbonate)-lithium bis (trifluoromethanesulfonyl) imide-ionic liquid solution for use in LIBs [162].", "It is showed that the mechanical stability and freestanding of composite membranes are improved by the reinforcing effect of silica NFs homogeneously into polymer matrix.", "Furthermore, conductivity of 10−5 S·cm−1 at 80 °C and favorable Li transference number of 0.36 are other achievements of using electrospun SiO2 NFs in LIB application.", "In another work, which assigned SiO2 NPs inside the electrospun P(VdF-HFP) NFs [163], it is concluded that in-situ incorporation of SiO2 NPs improves the electrical properties more than that achieved by directly mixing of silica to the polymer.", "Maximum ionic conductivity of 8.06 mS·cm−1 at 20 °C was achieved with 6% in situ silica.", "Appropriate electrolyte uptake (>550%) by high porosity (∼90%) electrospun membrane is another advantage of these materials in LIBs.", "Electrospun hybrid P(VdF-co-CTFE) and Al2O3 composite membrane made by Lee et al. [86] has been used in LIBs.", "It is found that thermal stability and cycling performance enhanced due to effective encapsulation of the electrolyte solution into good microporous structure of electrospun membranes.", "In another work to explore the effect of ceramic composite separators on the thermal shrinkage and electrochemical performance of the separators in LIBs, a nano sized Al2O3 coating was applied on both sides of microporous polyethylene (PE) separator [164].", "It is worth mentioning that the immiscible coating solution presents superior electrochemical performance, whereas the miscible coating solution shows the better thermal shrinkage.", "Furthermore, the microporous structure of ceramic coating affects the thermal shrinkage as well as the electrochemical performance of ceramic composite separators.", "The electrochemical performance of the electrospun ZnO/SnO2 composites for use as anode materials in LIBs has been investigated by Luo et al. [75] with regard to the effect of heat treatment on the efficiency of charge and discharge capacities.", "They found that calcination at 700 °C not only delivered high initial discharge and charge capacities of 1450 and 1101 mAh·g−1, respectively, with a 75.9% coulombic efficiency, but also maintained a high reversible capacity of 560 mAh·g−1 at a current density of 0.1 Ag−1 after100 cycles.", "In the other work that suggests improvements in the chemical properties of Ge-based anode materials, composite GeO2/SnO2 NFs were investigated for LIB application.", "It is found that GeO2 concentration has impact on enhancement of cycle stability of NFs as an anode.", "At the optimized concentration (Ge/Sn: 0.88), high initial reversible capacity of 922 mAh·g−1 and excellent cyclability (charge capacity retentions ~73.9%) were achieved [39].", "The room temperature ionic electrolyte made by electrospinning method is an alternative for the replacement of organic electrolytes.", "Raghavan et al. [91] examined nano-sized ceramic fillers (SiO2, Al2O3 or BaTiO3) hosted in electrospun P(VdFHFP) membranes for use in high energy density LIBs as a polymeric electrolyte.", "It is observed that composite ceramic NPs/Polymer NFs have good interfacial stability and oxidation stability at 5.5 V, and it is elucidated that the highest achievable potential of 6 V is belonged to membrane including BaTiO3 NPs.", "Furthermore, in comparison to the other membranes, this membrane delivered high initial discharge capacity of 165.8 mAh·g−1, which corresponds to 97.5% utilization of active material under the test conditions and showed the capacity fade after prolonged cycling.", "In another work, the incorporation of ceramic fillers (SiO2 and TiO2) inside a thermoplastic polyurethane (TPU)/PDdF based gel polymer electrolytes for LIB was studied.", "Based on the high ion conductivity (4.8 × 10−3 S·cm−1) and mechanical performance (8.7 ± 0.3 MPa) at room temperature, Wu et al. [165] suggest that TiO2 is more efficient in improving the properties of gel polymer electrolyte for practical application.", "In another research, Shim et al. [42] introduced electrospun LaCoO3 NFs for oxygen reduction and evolution in rechargeable Zn–air batteries.", "They explained that the LaCoO3 NFs have better electrochemical properties compared with the LaCoO3 powder, which is attributed to the increased surface area and number of active sites in the fibers. 5.7.", "Electronic Devices Electrospun NFs have the potential to be used in many electronic devices due to their high surface area, open porous microstructure and multi-composition.", "Hence, there are many efforts to discover new advanced materials fabricated via electrospinning method based on the electric and magnetic properties.", "Schutz et al. [37] could successfully create Cu2ZnSnS4 (CZTS) phase via electrospinning procedure and post heat treatment.", "The NFs characterization confirms the microstructure, composition and morphology of a homogeneous compact film, as is required for the production of photovoltaic cells.", "In other research, Ghashghaie et al. found that the electrospun ZnO NFs are capable to assemble into the inter-electrode space via dielectrophoresis force in above of 1 kHz (5 and 20 kHz) frequencies.", "Therefore, it is observed that ZnO NFs are aligned along the electric field lines thereby indicating desirable conditions for electronic device applications [21]. 5.8.", "Supercapacitors and Energy Harvesting Systems The development of renewable and sustainable energy sources is one of the main topics of recent researches due to decline of natural resources.", "Among the energy storage systems, supercapacitors and energy harvesting systems have specific attentions.", "Carbon-based NFs have been considered promising electrodes for advanced electrical energy storage systems, e.g., rechargeable batteries and supercapacitors, because of their high conductivity, good mechanical integrity, and large surface area [166].", "Hence, Wang et al. [29] applied electrospun CNFs substrates coated with a uniform ceramic MnO2 ultrathin layer by dip coating method for using in electrochemical capacitors.", "Based on the characteristics obtained for composite electrode (specific capacitance ~557 F·g−1), good rate capability and long-term cycling stability were observed.", "It is suggested that CNFs/MnO2 nanocomposites are promising for high-performance supercapacitors.", "In contrast, in another research, it was found that the best energy harvesting performance is obtained for pure PVDF NFs, with power outputs up to 0.02 μW and 25 μW under low and high mechanical deformation.", "Composite making with BaTiO3 NPs results in reduction of power output.", "It is because of enhancement of mechanical stiffness.", "It is suggested that the power output of the composites being better for the nonpiezoelectic smaller fillers [93].", "However, in accordance with the results obtained by Baji et al. [167], piezoelectric hysteresis and ferroelectric switching behaviors of electrospun (BaTiO3)/(PVDF) composite NFs are recognized.", "They investigated ferroelectric properties of the above-mentioned NFs by using piezoresponse force microscopy and found the polarization-voltage and amplitude-voltage hysteresis loops for (BaTiO3)/(PVDF) NFs. 5.9.", "Magnetic Parts Electrospinning procedure enables the facility to obtain nanocrystalline materials that have particularly important effects on magnetic materials.", "Recently, optimistic findings have been published throughout the electrospun magnetic NFs.", "Yensano et al. [45] studied the magnetic properties of electrospun La0.7Sr0.3MnO3 and they found that the specific saturation magnetization (Ms) value of calcined NFs at 900 °C is 40.52 emu·g−1 at 10 kOe.", "The increase of Ms is consistent with the enhancement of crystallinity and crystallite size by considering a magnetic domain of the samples.", "In another work, the magnetic properties of Ce0.96Fe0.04O2 NFs were investigated by S.", "Sonsupap et al. [33].", "It is found that as-spun samples (PVP/Ce0.96Fe0.04O2) exhibit a diamagnetic behavior, whereas the calcined Ce0.96Fe0.04O2 samples at 500–800 °C is ferromagnetic with the specific magnetizations of 0.002–0.923 emu·g−1 at 10 kOe.", "Hence, it is suggested that the electrospun Ce0.96Fe0.04O2 NFs can be further developed for many applications including ferrofluids, magnetic recording, biomedicine, and spintronics.", "Furthermore, Liu et al. [25] prepared BaFe12O19 fibers and hollow fibers by electrospinning and coaxial electrospinning method, respectively.", "They elucidated that the hollow NFs had low coercivity values of a few hundred Oersted while NFs have more than a thousand Oersted.", "They also found that the hollow NFs exhibited strong magnetism and basically showed soft specification.", "It is suggested that BaFe12O19 hollow NFs are promising for use in a number of applications, such as switching and sensing, electro-magnetism, and as microwave absorbers. 5.10.", "Dielectrics Ceramics are used in many electromagnetic interference shielding applications due to their appropriate dielectric characteristic.", "Electrospun products have a significant role in achieving multifunctional dielectric materials.", "In a study, the real and imaginary permittivity of carbon NFs was increased 3.5 times by incorporation of ZrO2 NPs, and the best efficient electromagnetic interference shielding effect (31.79 dB in 800–8500 MHz) is achieved when the amount of ZrO2 NPs is increased and heat treatment is carried out at 2100 °C [88].", "In other research, Qin et al. [30] found that CaCu3Ti4O12 NFs fabricated by standard electrospinning has a different dielectric constant from those synthesized by conventional bulk methods.", "It is suggested that NFs not only provide a new topic for investigation, but also supply new high-performance devices in electronic applications. 5.11.", "Thermoelectric Materials Composite NFs fabricated via electrospinning generate advanced materials for the conversion of waste heat into electricity as thermoelectric materials, due to enhanced phonon scattering at the nano-grain boundaries.", "Thermoelectric figure of merit (ZT) of electrospun boron-doped barium-stabilized bismuth-cobalt oxide have been studied by Cinar et al. [28].", "The physical measurement system values showed that the electrical and thermal conductivity, the Seebeck coefficient, and the ZT increased with the temperature rise.", "In contrast, they found that the ZT values decreased with doping of B.", "In other words, boron doping had a negative effect on the thermoelectric Ba-Bi-Co-O system.", "Thermoelectric and humidity sensing analysis of electrospun La2CuO4 NFs are also carried out by Hayat et al. [43].", "Their findings in the analysis of Seebeck and the analysis of impedance of La2CuO4 NFs indicated that the Seebeck coefficient increased from ∼30 to ∼300 μV·K−1 at 298–308 K, and the space-charge polarizations easily followed the changing direction of the electric filed at 100 Hz.", "They confirmed that the narrow adsorption-desorption hysteresis, short response and recovery time, excellent repeatability, high stability and high sensitivity of La2CuO4 NFs originated from a high surface to volume ratio of electrospun NFs, which enable them to be used as a humidity sensors. 5.12.", "Conductive Wires The advances in electrospun ceramic nanowires have brought an increasing interest in the potential technological applications such as those mentioned above as well as light-emitting diodes (LEDs), flexible displays, solar cells, organic LEDs, touch screens, and bio-textiles.", "Conductive fillers and metal conductive particles filled with flexible substrates can be easily formed by electrospinning method, such as silver NWs/PET, indium tin oxide (ITO)/PES, MWCNT and single wall carbon nanotubes (SWCNTs) [168].", "Conductive electrospun products show promising applications in various tissue engineering because of their higher conductivity.", "The neural tissue engineering is improved with the PPy, PANi and PEDOT fibrous conductive scaffolds.", "Also, conductive materials such as PPy, PANi, PLGA/CNF, CNTs and CNTs coated electrospun products are successfully utilized as scaffold materials for cardiac tissue engineering [169,170].", "Gaminian et al. [171] fabricated cellulose NFs decorated with Ag NPs by electrospinning followed by the deacetylation method.", "They believed that multi-functional cellulose NFs that are achieved by this method would provide biodegradable materials for various applications with a minimal amount of potentially toxic materials.", "Furthermore, not only is the electrical resistivity of cellulose NFs decorated with Ag NPs low (around 35 KΩ per square) but also their tensile strength is 87% higher than pristine cellulose NFs.", "There are a lot of reports on semiconductor NWs exploring excellent sensing properties due to high surface area.", "However, the sensing ability can be promoted by modification of morphologies.", "Liu et al. [172] explored that acetone sensitivity based on In2O3 nanotubes (NTs) is better than corresponding solid NWs.", "They suggest that the one-dimensional NT is probably a better candidate than NW for the higher response in the actual applications.", "On the other hand, pure and single phase ceramic NWs have also different performance than ceramic/polymer NWs.", "Chiu et al. [173] synthesized CuCrO2 NWs by electrospinning method.", "They found that the calcination conditions play a significant role in achieving single phase CuCrO2 NWs for use in p-type transparent optoelectronic devices. 5.13.", "Wearable and Electronic Textiles Nowadays, rapid developments in nanotechnology create a new application of electronic devices that are miniaturized to the point where embedded wearable applications are beginning to emerge [174].", "Electrospinning is one of the methods for production of wearable, smart and electronic textiles with multi functionality, flexibility, conductivity, low energy consumption, and miniaturization [175].", "Wearable mats are electronic and smart textiles that represent a useful feature for power management, and many electronic devices, fabrics, and bio-tissues will have to meet special requirements concerning wearable textiles [176].", "It is worth mentioning that wearable textiles are an innovate approach for converting mechanical movements to electrical power, and undoubtedly they will come to the market based on the recent successful results obtained by pioneer researchers.", "Hu et al. [177] successfully immobilized Ag NPs into electrospun Na-alginate NFs via a novel, cost-effective and antibacterial approach for using as flexible electronic skin.", "They explained that stable response of Ag/alginate nanofibrous membrane is because of uniform distribution of Ag NPs inside the alginate NFs.", "The electrospinning method provides conditions for them to synthesize the practical wearable electronic textiles that have an ultralow detection limit of 1 Pa and high durability more than 1000 cycles.", "Therefore, they suggest that electrospun Ag/alginate can be used as a pressure sensor on uneven human skin to sense respiration and vocal cords vibrations.", "A recent interest in the utilization of electrospun wearable electronic NFs is transparent human hair-based textiles.", "This is because of their unique optical properties in the visible light region.", "In order to apply wearable electronic devices with transparent textiles, Lee et al. [178] fabricated transparent ZnO/graphene quantum dots textiles via electrospinning method and found that the luminescence of these textile LEDs devices is ~70.19 cd·m−2.", "Park et al. [179] successfully synthesized environmentally friendly human hair-based, transparent, keratin/PVA NFs via electrospinning method.", "They investigated a comparison between polymer light-emitting diodes (PLEDs) without textile and consolidated PLEDs with textile for study the transparency of NFs for wearable devices.", "The performance with a spectrally white, red and yellow color light of consolidated textile/PLEDs/textile devices indicated a maximum luminance of 2791, 2430, and 6305 cd·m−2, and a current efficacy of 0.29, 0.10, and 0.38 cd·A−1, respectively.", "Their findings indicate that consolidated wearable devices with the PLEDs embedded in the environmentally friendly transparent NF textiles opened a new world of applications for wearable electronics.", "Energy storage materials have significant roles in energizing portable and wearable electronics.", "Assessment of multi hierarchical constructions those fabricated via the electrospinning procedure enhance the ability of flexible supercapacitor electrodes.", "Activated carbon fibers such as flexible substrates, PANI and CNT as conductive materials can make a high performance mats for flexible textile electrodes that have good cycling stability, energy density and power density [180].", "Furthermore, piezoelectric materials respond to wearable smart textiles because they can convert mechanical energy into electrical energy through a piezoelectric effect.", "The piezoelectric properties of PVDF NFs embedded BaTiO3 NPs have been evaluated toward NPs concentration by Lee et al. [92].", "Their findings showed that the magnitude of the resultant voltage increases as the NPs concentration increases.", "The piezoelectric output voltages of PVDF/BaTiO3 were 1.7 times greater than single phase PVDF NFs.", "Moreover, uniaxially-aligned PVDF/BaTiO3 NFs suggest possible uses in energy harvesting and as power sources in miniaturized electronic devices like wearable smart textiles and implantable biosensors.", "The next generation wearable textiles will belong to nanofibrous membranes that are capable of converting human biomechanical energy into electricity.", "Some efforts are under development to construct bio electric nanogenerators.", "This is of vital importance to portable energy-harvesting and personal electronics.", "Electrospinning provides portable, and wearable self-powered nano/microsystems that require the piezoelectric materials to be flexible and lightweight.", "Li et al. [181] have demonstrated that the electrospun nanofibrous membranes are tailored to enhance the polarity, mechanical strength as well as surface hydrophobicity of bio electric nanogenerators, which will eventually improve the device performance, power, and capability of operation even with high environmental humidity.", "Wu et al. [175] synthesized a textile with parallel NWs of lead zirconate titanate (PZT) by electrospinning method for using it into flexible and wearable nanogenerators.", "The electrospun PZT NWs can generate an output voltage of ~6 V and output current of ~45 nA, which are large enough to power a liquid crystal display and a UV sensor, as well as powering wearable microsystems [174]. 5.14.", "Other Applications Similar to the common fibers which are applied for reinforcing the bulk materials, electrospun NFs are also used to increase mechanical strength.", "Calleja et al. [26] prepared a thin film of YBa2Cu3O7−x embedded electrospun fiber network of BaZrO3 and investigated this for mechanical strength.", "They found that mechanical performance of the composite enhanced due to the presence of NFs.", "Not only a mechanical reinforcement, but also other interesting composite materials can be designed based on the using electrospun NFs.", "Electrospun SiO2 NFs have been examined as coating to the ceramic tile surfaces.", "It is worth mentioning that by electrospinning technique, microscopic defects of tile surface can be covered with NFs [56].", "In a different application of electrospun ceramic NFs, hybrid configuration of nafion/silica NFs were examined for fire resistance properties and wettability.", "It is found that not only were the thermal properties of nafion enhanced by chemical bonding with silica NFs, but also fire resistance improved with porosity features, which could effectively prevent fire speed and heating flow.", "In organic–inorganic sols, the phase rearrangement is induced by applied high voltage field, which leads to highly conductive polymer being forced to the surface of composite fiber to form shell to protect the inner inorganic materials [182].", "According to the sound absorption properties of electrospun mats, Gao et al. [183] assigned electrospun PVA/TiO2 and PVA/ZrC composite mats for using a spiral vane electrospun machine.", "They carried out the sound test in the impedance tube at the frequency range from 500 to 6500 Hz.", "It is found that sound absorption properties of composite shifted to a higher frequency region when ZrC NPs loaded, and better sound absorption properties seen above 2500 Hz with increasing content of ZrC.", "For TiO2 NPs, the size of NPs is the main variable in terms of adsorbing sound.", "Therefore, it can be said that the NPs had an effect on sound absorption materials, with different types and sizes, and sound absorption properties will improve in different ranges of frequency.", "The reducibility of the electrospun CexSm1−xO2 NFs as well as their thermal stability in successive oxidation–reduction cycles has been evaluated in H2 atmosphere by Jaoude et al. [34].", "They found that the CexSm1−xO2 NFs have mobile oxygen species (reducible sites) and a wide range of acid/basic sites.", "Furthermore, the CexSm1−xO2 NFs enhanced the reactive adsorption of ammonia leading to the production of NH3, NO, N2O and N2O species.", "According to the obtained results, they suggest CexSm1−xO2 NFs for use in energy-related industrial applications such as hydrocarbons steam reforming, water gas shift reaction and cracking reactions. 6.", "Summary and Future Perspectives Ceramic NFs can be synthesized via several methods.", "However, the electrospinning method has significant advantages over the others because it is straightforward, cost-effective, and versatile and can produce ceramic fibers in the nanometers to micrometers range.", "Utilization of ceramic NFs instead of bulk ceramics improves the performance of devices due to special properties that come from electrospinning products.", "Electrospinning is a practical method to produce ceramic fibers in a variety of shapes: one dimensional, tubular, hollow, core-shell, and porous.", "Not only the shapes of fibers, but also tha pattern of fibrous mats can be changed via electrospinning procedure: non-woven, cross and aligned fibers, 3D mats and ropes.", "Single phase ceramic fibers are synthesized by calcination of electrospun hybrid ceramic/polymer fibers.", "Polymer has significant role to obtain appropriate viscosity for pre-spinning solution.", "PVA and PVP are fairly common polymer reagents for the above-mentioned purpose.", "By reviewing recent developments in electrospun ceramic NFs, it is found that not only can simple oxide ceramic fibers such as, Al2O3, MgO, SiO2, TiO2, ZnO and ZrO2 be fabricated via electrospinning method, but also complex oxide ceramic fibers such as CaCu3Ti4O12 and Li1.6Al0.6MnO4 can be easily synthesized.", "The surface activity of ceramic NFs can be improved by post treatment like pyrolysis, hydrothermal and carbothermal processes.", "The integration of electrospinning with surface modification procedure presents a pioneering method for fabrication of complex non-oxide ceramic NFs (e.g., Cu2ZnSnS4), high crystallized fibers, and they are never synthesized via other methods.", "With the decrease in diameter and length of a fiber, many properties of fibrous materials are modified, and characterization of NFs seems to be different from bulk materials.", "For example, the zeta potential of ceramic NFs are measured by the different procedure and setup compared to the one for powders and common materials.", "The recent findings have shown the great potential of electrospun ceramic NFs to be used for making various catalyst parts, filtration media, sensors, electronic devices, magnetic parts, wearable electric textiles, and biomedical ones.", "We can summarize recent ceramics NFs synthesized via electrospinning in following list according to their applications. ■ Catalysts: TiO2, V2O5, ZnO, SnO2, CdTiO3, Bi2MoO6, Nb2O5, Gd2O3 ■ Filtration: TiO2, Al2O3, Clay, Fe3O4, SrFe12O19 ■ Biomedical: HA, CaO, SiOC, TiO2, ZnO ■ Fuel Cells: Pr0.4Sr0.6Co0.2Fe0.7Nb0.1O3−δ, GdBaCo2O5+δ ■ Sensors: SnO2, ZnO, TiO2, CeO2, NiO, LaMnO3 ■ Batteries: SiO2, Al2O3 SnO2, GeO2, BaTiO3, LaCoO3 ■ Electromagnetic devices: Cu2ZnSnS4, ZnO, BaO, La0.7Sr0.3MnO3, Ce0.96Fe0.04O2, BaFe12O19, CaCu3Ti4O12, ZrO2, La2CuO4 ■ Energy harvesting and capacitors: BaTiO3, MnO2, In2O3 ■ Wearable electric textiles: ZnO, Geraphene, CNT, BaTiO3, PZT ■ Other applications: Al2O3, BaZrO3, SiO2, ZrC, CexSm1−xO2 It should be noted that above list does not include all progress around the world: there are definitely now many efforts being studied in research laboratories, and with further progress in electrospinning techniques, electrospun ceramic NFs will come into the market and be utilized in many devices in the not-too-distant future." ]

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[ "Study on Zinc Oxide-Based Electrolytes in Low-Temperature Solid Oxide Fuel Cells Study on Zinc Oxide-Based Electrolytes in Low-Temperature Solid Oxide Fuel Cells https://orcid.org/0000-0002-3133-7031XiaChen13QiaoZheng12FengChu1 https://orcid.org/0000-0002-3696-7251KimJung-Sik4WangBaoyuan1*ZhuBin13* 1Hubei Collaborative Innovation Center for Advanced Organic Chemical Materials, Faculty of Physics and Electronic Science, Hubei University, Wuhan 430062, China; cxia@kth.se (C.X.); qiaozheng@hgnu.edu.cn (Z.Q.); musia0803@163.com (C.F.) 2College of Mechanical and Electrical Engineering, Huanggang Normal University, Huanggang 430062, China 3Department of Energy Technology, KTH Royal Institute of Technology, 10044 Stockholm, Sweden 4Department of Aeronautical & Automotive Engineering, Loughborough University, Loughborough LE11 3TU, UK; J.Kim@lboro.ac.uk *Correspondence: baoyuanw@163.com (B.W.); binzhu@kth.se or zhubin@hubu.edu.cn (B.Z.) 40 Semiconducting-ionic conductors have been recently described as excellent electrolyte membranes for low-temperature operation solid oxide fuel cells (LT-SOFCs).", "In the present work, two new functional materials based on zinc oxide (ZnO)—a legacy material in semiconductors but exceptionally novel to solid state ionics—are developed as membranes in SOFCs for the first time.", "The proposed ZnO and ZnO-LCP (La/Pr doped CeO2) electrolytes are respectively sandwiched between two Ni0.8Co0.15Al0.05Li-oxide (NCAL) electrodes to construct fuel cell devices.", "The assembled ZnO fuel cell demonstrates encouraging power outputs of 158–482 mW cm−2 and high open circuit voltages (OCVs) of 1–1.06 V at 450–550 °C, while the ZnO-LCP cell delivers significantly enhanced performance with maximum power density of 864 mW cm−2 and OCV of 1.07 V at 550 °C.", "The conductive properties of the materials are investigated.", "As a consequence, the ZnO electrolyte and ZnO-LCP composite exhibit extraordinary ionic conductivities of 0.09 and 0.156 S cm−1 at 550 °C, respectively, and the proton conductive behavior of ZnO is verified.", "Furthermore, performance enhancement of the ZnO-LCP cell is studied by electrochemical impedance spectroscopy (EIS), which is found to be as a result of the significantly reduced grain boundary and electrode polarization resistances.", "These findings indicate that ZnO is a highly promising alternative semiconducting-ionic membrane to replace the electrolyte materials for advanced LT-SOFCs, which in turn provides a new strategic pathway for the future development of electrolytes. semiconducting-ionic conductor solid oxide fuel cells zinc oxide composite electrolyte proton conduction 1.", "Introduction In the preceding decades, fuel cells (FC) technologies have attracted enormous attention for power generation due to the imperious demand of humankind for sustainable energy resources [1,2].", "As a typical category of FC technologies, solid oxide fuel cells (SOFCs) are currently receiving ever-increasing research interest because of their distinguishing advantages of high energy conversion efficiency, low greenhouse gas emissions and excellent fuel flexibility [3,4,5].", "Unfortunately, current high-temperature SOFCs suffer from high manufacturing costs and technological complexities, due to the fact that yttria-stabilized zirconia (YSZ) electrolyte requires high temperatures (800–1000 °C) or precisely controlled thin film quality by advanced technologies to reach a sufficient ionic conductivity [6,7].", "On the other hand, intermediate-temperature (600–800 °C) SOFCs are subject to an issue regarding the reduction reaction of Samarium-doped ceria (SDC) electrolyte in hydrogen atmosphere, which introduces additional electronic conduction and thus results in serious power loss to the cell [8].", "Therefore, to realize the widespread application of SOFCs, it is highly critical to overcome the barriers of high-temperature operation and material degradation to develop advanced low-temperature (300–600 °C) SOFCs (LT-SOFCs).", "Since the electrolyte layer is well known as the heart of a fuel cell device in determining the operational temperatures and durability as well as the ultimate energy conversion efficiency, new strategies for excavating alternative electrolytes with high and stable ionic conductivity at reduced temperatures are strongly desired.", "To address this challenge, an efficacious approach based on semiconducting ionic conductors has been proposed very recently to replace the conventional electrolyte YSZ and SDC [9,10,11,12,13,14,15].", "The developed materials have exhibited extraordinarily high ionic conductivity superior to those of YSZ and SDC, showing tremendous potential as membrane layer in LT-SOFCs [14,15].", "For instance, a breakthrough study on SmNiO3 reported a high protonic conductivity in such perovskite semiconductor that compare favorably with those of best-performing solid electrolytes.", "The corresponding SOFC with Pt/SmNiO3/Pt geometry demonstrated dramatic power output of 225 mW cm−2 at 500 °C [16].", "Tao et al. also demonstrated that good proton conduction (0.1 S cm−1 at 500 °C) can be obtained in semiconductor LixAl0.5Co0.5O2 [17].", "Our previous work also detected high ionic transport in a natural hematite (α-Fe2O3) and applied the semiconducting hematite electrolyte into SOFC, observing an impressive power density of 467 mW cm−2 at 600 °C [18,19].", "In addition to these single phase semiconductors, high ionic conduction is also found in hetero-structured materials.", "Garcia-Barriocanal et al. reported a colossal ionic conduction at the interfaces of ionic conductor/semiconductor hetero-structure YSZ/SrTiO3, indicating that substantial ionic conductivity can be achieved even close to room temperature [20].", "A series of composite materials consisting of semiconductors and ionic conductors such as Li0.15Ni0.45Zn0.4Ox/SDC and SDC/Na2CO3-Sr2Fe1.5Mo0.5O6−δ were also applied as membranes in SOFCs, revealing significantly enhanced ionic conductivity as compared to single phase ionic conductors [21,22,23,24].", "A new fuel cell technology, named as electrolyte-layer free fuel cell (EFFC) or semiconductor-ion membrane fuel cell (SIMFC) designed by energy band alignment and perovskite solar cell principle has been proposed to realize better integration and functionality of these materials [11,14].", "Such type of cell device is assembled using Ni0.8Co0.15Al0.05Li-oxide (NCAL) as electrodes into a typical configuration similar to perovskite solar cell: NCAL (ETL)/semiconducting ionic conductor (function layer)/NCAL (HTL) (ETL and HTL mean electron transport layer and hole transport layer), managing to achieve better fuel cell performances in a simpler device architecture [22].", "The semiconductor ZnO has gained substantial interest in the research community and industrial applications because of its peculiar properties, such as excellent thermal stability, good oxidation resistance, considerable optoelectronic properties, and band gap in the near ultraviolet [25].", "It is well known not only as a versatile semiconductor but also as a probable oxygen-ion conductor due to the enrichment of oxygen vacancies at high temperature [26].", "It has been reported that the oxygen vacancy is a deep donor in ZnO with a (2+/0) transition level at ~1.0 eV below the bottom of the conduction band [27].", "Liu et al. observed that addition of 0.5 wt % ZnO increased the ionic conductivity of YSZ by as much as 120% at 800 °C [28].", "Furthermore, protons also may exist in ZnO and doped ZnO due to the fact that hydrogen is easily ionized to protons in oxide lattice.", "As reported, it is detected the concentration of protons in ZnO increases with elevating temperature [29].", "Economically, ZnO is a cost-effective material in practical applications, for that it is able to be synthesized by remarkably simple crystal-growth technologies.", "Therefore, taking advantage of the properties of ZnO and following the above strategy, this work accesses the utility of ZnO-based materials for electrolytes in LT-SOFC.", "Two types of fuel cells are fabricated using pure ZnO and ZnO-LCP (La/Pr-doped CeO2) composite as membrane layer, respectively, sandwiched between two NCAL electrodes.", "The structure, morphology and electrical properties of the materials are investigated.", "The performances of the cells are evaluated within a low temperature range of 450–550 °C. 2.", "Experimental Section ZnO powders were obtained through a simple pre-sintering of commercial ZnO at 650 °C for 2 h.", "The sintered powders were ground thoroughly for electrolyte uses and further composite preparation.", "LCP (La0.33Ce0.62Pr0.05O2−δ) powder was synthesized through an 800 °C heat treatment of LaCePr-carbonates, which is a mixture of lanthanum, cerium, and praseodymium carbonates.", "Afterwards, ZnO-LCP composite was prepared by blending the sintered ZnO with LCP in a mass composition of 1:1.", "The resultant mixture was heated again at 800 °C for 2 h and ground completely to obtain the eventual homogeneous ZnO-LCP composite material.", "The commercial ZnO was purchased from Sigma Aldrich, Shanghai, China, and the raw material LaCcPr-carbonate was obtained from a rare-earth company in Baotou, China.", "Additionally, the electrode material NCAL was processed in a slurry form by mixing NCAL powder with terpineol solvent.", "The resultant slurry was pasted onto Ni-foam and desiccated at 120 °C for use as an electrode and current collector.", "The commercial NCAL was purchased from Tianjin Bamo Science and Technology Joint Stock Ltd., Tianjin, China.", "Regarding the fabrication of fuel cells, two fuel cell devices were assembled based on ZnO electrolyte and ZnO-LCP composite, respectively, with two pieces of Ni-foam pasted by NCAL on both sides in each case; subsequently the three layers were pressed uniaxially under a load of 200–250 MPa into one tablet.", "For comparison purpose, a device based on LCP electrolyte was also fabricated in the same configuration.", "The resulting fuel cell devices, NCAL/ZnO/NCAL, NCAL/ZnO-LCP/NCAL, and NCAL/LCP/NCAL are roughly 2 mm in thickness and 13 mm in diameter (active area of 0.64 cm2).", "All devices, were pre-treated using an in situ heating step at 600 °C for 1 h after being mounted into the testing setup, before performance measurements at 450–550 °C.", "The crystal structures of samples were studied using a Bruker D8 Advanced X-ray diffractometer (XRD, Bruker Corporation, Karlsruhe, Germany) with Cu Kα (λ = 1.54060 Å) as the source, with tube voltage at 45 kV and current of 40 mA.", "The particle morphology of powder samples, cross section and elemental composition of fuel cell device were investigated using a JEOL JSM7100F field emission scanning electron microscope (FE-SEM, Carl Zeiss, Oberkochen, Germany) under an accelerating voltage of 200 kV, and the equipped energy dispersive spectrometer (EDS, Carl Zeiss, Oberkochen, Germany) that operated at 15 kV.", "The electrochemical impedance spectra (EIS) of fuel cells were measured in H2/air atmosphere using an electrochemical work station (Gamry Reference 3000, Gamry Instruments, Warminster, PA, USA).", "The measurement was performed under open circuit voltage (OCV) conditions, and the applied frequency range was 0.1–106 Hz with a AC signal voltage of 10 mV in amplitude.", "The performance measurements for fuel cells were carried out on a programmable electronic load instrument (IT8511, ITECH Electrical Co., Ltd., Nanjing, China) at 450–550 °C with humidified hydrogen as fuel (120–140 mL min−1) and air as the oxidant (120–150 mL min−1). 3.", "Results and Discussion 3.1.", "Crystalline Structure and Morphology The XRD patterns of the prepared ZnO, LCP and ZnO-LCP composite are presented in Figure 1.", "The XRD of ZnO displays a series of characteristic diffraction peaks that correspond to the (100), (002), (101), (102), (110), (103) and (112) planes in JCPDS File No. 36-1451, which can be well indexed to the typical hexagonal wurtzite structure of zinc oxide [30].", "The XRD diagram of LCP is characteristic of a cubic fluorite structure, with a slight shift to lower angle compared with the standard pattern of ceria (JCPDS File No. 34-0394), echoing the fact that LCP is a La/Pr co-doped CeO2 as reported previously [31].", "In the diffractogram of ZnO-LCP composite, all diffraction peaks emerged can be assigned to wurtzite phase of ZnO and cubic fluorite phase of LCP, no extra phases and peak shift could be identified, which confirms that no chemical interaction occurred between the two materials.", "Compared to the XRD patterns of ZnO and LCP, the composite sample shows less intense peaks, revealing a larger full width at half maximum (FWHM) of the characteristic peak.", "According to the Scherrer equation D = K γ Bcos θ, it can be calculated that the average grain size (D) of the material decreased from 26 (ZnO) and 15 (LCP) to 12 nm (ZnO-LCP).", "Moreover, the interplanar spacing values and lattice parameters of ZnO and LCP from the XRD analysis are given in Table 1.", "The micro-structure of the resultant materials and fuel cell device were investigated by SEM.", "Figure 2a,b shows the recorded morphology of ZnO particles and ZnO-LCP particles.", "As can be seen, both ZnO and ZnO-LCP exhibit nano-sized particles and irregular shape particles, which is owing to the utilization of commercial and industrial-grade materials without elaborate control of nano-structure, while the composite material appears to be made up of more condensed particles with better distributions.", "Moreover, the average grain/particle size of ZnO-LCP were found to be smaller than that of ZnO, which is in good agreement with the XRD result.", "The observed size values are larger than the calculated grain size results according to the Scherrer equation, indicating that small grains aggregated in the materials and formed larger particles.", "Figure 2c illustrates a cross-sectional SEM image of the NCAL/ZnO-LCP/NCAL cell after operation, clearly displaying three individual layers consisting of a membrane layer with thickness of 550 μm and two porous NCAL-Ni electrode layers.", "The ZnO-LCP membrane layer adheres well with the NCAL-Ni layer without any delamination trace even after scissoring treatment for SEM characterization, as an indication of satisfactory mechanical strength of the device.", "Three high-magnification images of the NCAL-Ni layer, NCAL particles and the intermediate layer are further presented in Figure 2d,e, respectively.", "Figure 2d shows a clear view of the NCAL particles located in the three dimension woven structure of Ni-foam, forming a porous structure, which is ulteriorly confirmed in Figure 2e.", "The particle size of NCAL ranges from 50 to 200 nm.", "Additionally, as the core component of the fuel cell, ZnO-LCP layer exhibits a gas-tight structure in Figure 2f while no distinct sign of cracking can be observed.", "Apart from blocking gas leakage/crossover during operation, this dense layer can also ensure fast ion transport and thus aid in reducing the internal resistance of the single cell.", "In order to study the compatibility of the cathode and electrolyte membrane materials, Figure 3a presents a SEM image of the NCAL/ZnO-LCP/NCAL cell focusing on the membrane/cathode interface region after operation, and Figure 3b gives a detailed morphology on the basis of Figure 3a, which verifies the dense layer of ZnO-LCP membrane and porous structure of cathode again.", "The elemental mappings for Zn (elements only from membrane) and Ni (element only from electrode) in Figure 3c,d clearly distinguish the interface between membrane and cathode.", "These results indicate that ZnO-LCP membrane layers were well bonded with the NCAL cathode layer during operations without any interlaminar separation or fissure, revealing a good thermal compatibility between the membrane materials and cathode materials.", "Figure 3e–h further give the EDS analysis results based on the cross-section of the ZnO-LCP cell after operation.", "The borders between membrane layer and electrode are clear and uniform, confirmed by the elemental mappings of Zn, Ce and Ni.", "It reflects that there was no obvious elemental interdiffusion or segregation occurred at the interfaces during operation, which excludes the possibility of any undesired secondary reaction, and thus confirms the good chemical compatibility of the electrode and electrolyte materials. 3.2.", "Electrochemical Performance Figure 4 shows the typical current-voltage (I-V) and current-power (I-P) characteristics for the three fuel cells based on ZnO, LCP, and ZnO-LCP electrolytes, respectively at 550 °C.", "From Figure 3a, it can be observed that ZnO cell delivers an OCV of 1.06 V and a maximum power density of 482 mW cm−2, slightly lower than that of LCP cell with 540 mW cm−2 in peak power density.", "This is the first demonstration of ZnO in fuel cell device that shows considerable performance at low temperature.", "It suggests the tremendous potential of ZnO from scientific and technological as well as applied perspectives for electrolyte uses.", "We also note that the performance is comparable to that of a newly reported thin-film SOFC based on YSZ/GDC (Gd-doped CeO2) bi-layer electrolyte [32], and even superior to some other SOFCs using ceria-based electrolytes [33,34].", "In the case of the ZnO-LCP cell, a higher OCV of 1.07 V and significantly enhanced power density of 864 mW cm−2 were attained at 550 °C compared to other two cells.", "The power output manifested an almost 2-fold increment over that of ZnO cell.", "This sharp enhancement is most likely explained by the enhanced ionic conductivity in ZnO-LCP composite through interfacial conduction effect, as confirmed formerly in a number of semiconducting ionic conductors [15,19,35,36].", "Based upon the above investigations, the ZnO-based cells were further assessed at reduced temperatures from 450 to 525 °C, with a 30-min dwelling time at each testing point to stabilize the cell.", "As shown in Figure 4b, the ZnO cell exhibits boosted power output from 158 to 380 mW cm−2 at 475 to 525 °C along with a mildly raised OCV from 1 to 1.03 V.", "Within the same temperature range, the ZnO-LCP cell demonstrates appreciable power outputs, reaching 390, 625 and 794 mW cm−2 at 475, 500 and 525 °C, respectively, while the OCV fluctuates in the 1.08~1.1 V window, as shown in the inset of Figure 4b.", "The enhancements of power density are mainly due to the thermally activated ion transport in Zno and ZnO-LCP with the rise in temperature.", "The achieved high OCVs can be ascribed to the excellent catalytic activity of NCAL, which has been reported as an efficient catalyst for both anode and cathode with superior triple O2−/H+/e− conduction [37], and the junction effect of the device [38].", "It needs to be emphasized that the junction effect is based on a Schottky junction formed between the Co/Ni alloy layer, which was originated from the anodic NCAL via reduction reaction, and the intermediate ZnO or ZnO-LCP semiconductor layer.", "The Schottky barrier field in the junction points from alloy layer to semiconductor layer, playing a crucial role in preventing electrons in H2 supply side from passing through the device [11,14].", "Consequently, though there is a significant electronic conduction in the ZnO-based electrolytes, high OCVs can be still obtained by the cells.", "In addition, the two cell devices were further operated at lower temperature, observed is that both cells failed to reach a sufficient OCV at 450 °C, which is chiefly due to the poor catalytic activity of the NCAL electrodes at too low temperatures [39].", "However, it still can be concluded from current initial results that both ZnO and ZnO-LCP composite can function well as electrolyte membrane layer in LT-SOFCs. 3.3.", "Electrical Conductivity To understand the excellent electrochemical performances of ZnO-based fuel cells, the conductivity of the used ZnO-based materials were studied.", "As reported, the linear part in the central region of I-V characteristic curve mainly reflects the ohmic loss of electrolyte in a SOFC [40,41], thus ohmic resistances of the ZnO and ZnO-LCP layer can be estimated from the slope of I-V curves, from which the ionic conductivity (σ) that contributes to cell performance can be calculated according to σ = L R × S, where L is the thickness of the electrolyte layer, S denotes the effective area, and R represents the resistance.", "Figure 5a shows the estimated ionic conductivities for the used ZnO electrolyte and ZnO-LCP composite as a function of temperatures.", "The ionic conductivity of ZnO is 0.037 S cm−1 at 475 °C and increases to 0.09 S cm−1 at 550 °C.", "This result is slightly ahead of those of well-known oxygen ion electrolytes YSZ, GDC, Mg-doped LaGaO3 (LSGM), and typical proton electrolytes BaCe0.5Y0.5O3−δ (BCY) and BaZr0.1Ce0.7Y0.2O3−δ (BZCY) in previous reports [42,43].", "ZnO-LCP reveals a significantly promoted ionic conductivity of 0.082 S cm−1 at 475 °C, which then reached as high as 0.156 S cm−1 at 550 °C.", "The corresponding activation energy (Ea) for ionic conduction can be obtained based on Arrhenius relationship σ = A T exp ( − E a kT ), in which T is the absolute temperature, A is a pre-exponential factor, and k represents the Boltzmann constant.", "As presented in Figure 5b, the Ea for ionic conduction of ZnO and ZnO-LCP at 475–550 °C are 0.7 and 0.51 eV, respectively, showing smaller values than those of pure O2− conductors YSZ and LSGM.", "Particularly, the Ea for ZnO is close to the reported activation energies of pure proton conductors BCY and BZCY, which are in the scope of 0.66–0.78 eV [44].", "Consider that protons in solid proton electrolytes generally require much lower activation energy to motivate their transport than oxygen ions, it is speculated that the ZnO-based electrolytes possess hybrid proton and oxygen ion conduction, thus resulting in a coupling lower Ea.", "To verify the speculation, an additional experiment was undertaken to test the proton conductive behavior of ZnO electrolyte by using a O2− blocking fuel cell in configuration of NCAL/BZCY/ZnO/BZCY/NCAL.", "Since BZCY is a state-of-the-art proton conductor with major proton conduction and negligible oxygen ion and electron conduction [45,46], the trilayer BZCY/ZnO/BZCY membrane would primarily transport protons from the anode side to cathode side while filtering out oxygen ions and electrons.", "By this means, the proton conductive property of ZnO can be confirmed from the performance of this multilayer cell device.", "This method has been reported for testing proton-related properties and conductivities of specific materials [47,48].", "Figure 6a illustrates the cross-section of the device characterized by SEM after performance measurements and the corresponding elemental mappings from EDS test.", "As can be seen, five layers of the NCAL/BZCY/ZnO/BZCY/NCAL architecture can be clearly distinguished in SEM.", "This is ulteriorly identified by the elemental mappings of Ni, Zn and Ba in Figure 5a, which are exclusive from the NCAL, ZnO and BZCY layer, respectively.", "Few cracks are detected in the two BZCY layer membranes, probably resulting from scissoring the cross-section for SEM measurement.", "Figure 6b shows the cell electrochemical performance at 550 °C, exhibiting a maximum power density of 235 mW cm−2 with an OCV of 1.05 V.", "This result reflects only proton transport contribution to the power output.", "Therefore, from the I-V curve the proton conductivity of ZnO was calculated to be 0.05 S cm−1 at 550 °C.", "Compared to the total ionic conductivity of ZnO (0.09 S cm−1 at 550 °C), this value (0.05 S cm−1 at 550 °C) indicates that the used ZnO electrolyte might be a hybrid O2−/H+ conductor, where proton conduction dominates the total ionic conduction.", "However, with the multilayer configuration, the additional layers and interfaces would induce more power losses, which means the calculated value for the proton conductivity is smaller than the actual value.", "Therefore, it is more likely that the used ZnO electrolyte is a pure proton conductor rather than mixed proton and oxygen-ion conductor, as reported in previous study [29].", "Such conductive behavior could account for the low activation energies of the materials.", "Our study thus confirms the proton conductive property of ZnO. 3.4.", "Impedance Spectroscopy Analysis Notably, the ZnO-based fuel cell exhibited significantly enhanced performance by incorporating ionic conducting LCP to form a composite.", "For comparative study of the electrochemical processes between our ZnO-based composite fuel cell and conventional doped-CeO2-based fuel cell, impedance spectroscopy analysis was carried out for the two types of cells.", "Figure 7 presents the EIS results of LCP cell and ZnO-LCP cell acquired in H2/air at 525 and 550 °C.", "In each impedance spectrum, the intercept with the real axis at high frequencies reflects the bulk resistance, the semicircle at intermediate frequencies represents the grain-boundary process, while the semicircle at low frequencies region corresponds to the electrode polarization behavior [41,49].", "An intuitive comparison from the curves indicates that the EIS for ZnO-LCP cell have smaller high-frequency intercepts and smaller semicircles than LCP cell.", "We employed an empirical equivalent circuit model of LRb(RgbQgb)(ReQe) to fit the EIS data to get internal resistances information, in which L is inductance of the instrument leads and current collectors, Rb, Rgb and Re stand for bulk resistance, grain boundary resistance and electrode polarization resistance respectively, and Q is the constant phase element (CPE) representing a non-ideal capacitor.", "Thereby, RgbQgb and ReQe denote the semicircles of grain boundary conduction and electrode polarization process, respectively.", "The simulated parameters extracted from the fitting results are summarized in Table 2.", "It can be discerned that the Rb of ZnO-LCP cell shows slightly smaller Rb than that of LCP cell at both 525 and 550 °C.", "With respect to the Rgb, ZnO-LCP exhibits evidently reduced values of 0.034 Ω cm2 (550 °C) and 0.045 Ω cm2 (525 °C) as compared to LCP.", "This partly manifests that the migration of ions at the grain boundary is less resistive in the composite.", "We attributed this phenomenon to the heterophasic interfacial conduction effect at semiconductor oxide/ionic conductor oxide interface regions in hetero-structured composite material [19,50].", "Such behavior has been reported in many semiconducting ionic systems, such as La0.6Sr0.4Co0.2Fe0.8O3−δ-Ca0.04Ce0.8Sm0.16O2−δ (LSCF-SCDC), YSZ-SrTiO3, and CoFe2O4-GDC [15,20,51].", "Furthermore, greater difference is observed between the Re of the two devices, whereby ZnO-LCP possesses smaller Re with values of 0.144 Ω cm2 at 550 °C and 0.197 Ω cm2 at 525 °C.", "Since these electrolyte/electrode interfacial polarization resistances often cause significant power losses in SOFCs, the smaller Re of ZnO-LCP would help in attaining higher power output of the cell.", "The above results regarding internal resistances commendably interpret the promoted performances in ZnO-LCP composite fuel cell.", "Figure 8 displays the EIS of ZnO-LCP measured in H2/air at various temperatures.", "The EIS curves present in a form of flat-shaped arc or semicircle, because of the mixed electron and ion conductive behavior in the composite.", "With the testing temperature increases from 475 to 550 °C, the bulk resistance drops slightly from 0.072 to 0.046 Ω cm2, while the polarization resistance which is reflected by the intercept of arc or semicircle on the real axis reveals a dramatic shrunken tendency.", "For instance, at 475 °C the polarization resistance of the cell is about 1.2 Ω cm2 whereas the bulk resistance is smaller by one order of magnitude.", "It is also noted that the polarization resistance at 475 °C are far greater than those at temperatures over 500 °C.", "This should arise from the fact that both catalytic activity of electrode and ionic conduction of electrolyte require a sufficient thermal condition to realize their functions, suggesting that the currently designed ZnO-based cells are more applicable to operate at over 500 °C.", "Clearly, on the one hand, the above results prove the operational feasibility of ZnO-based electrolyte fuel cells at LT.", "On the other hand, it signifies that the 300–475 °C LT operation of the cell remains a huge challenge, which requires more scientific and technological studies on the materials. 4.", "Conclusions In summary, two zinc oxide-based electrolyte materials, pure ZnO and ZnO-LCP composite, have been developed for LT-SOFC applications for the first time.", "The two types of fuel cells based on pure ZnO and ZnO-LCP composite exhibited excellent power outputs of 482 and 864 mW cm−2 at low temperature of 550 °C, respectively.", "On this basis, our investigation found that ZnO electrolyte possessed decent ionic conductivity of 0.09 S cm−1 at 550 °C along with activation energy of 0.70 eV, while ZnO-LCP composite exhibited promoted ionic conductivity of 0.156 S cm−1 at the same temperature with low activation energies of 0.51 eV.", "These results are ahead of some standard electrolytes in previous reports.", "More profoundly, the proton conductive property of ZnO was detected using an oxygen-ion blocking fuel cell, showing a considerable proton conductivity of 0.05 S cm−1 at 550 °C.", "Besides, the improved performance and electrochemical processes of the ZnO-LCP cell were investigated through impedance spectra measurements.", "The improvements are discovered to be majorly owing to the reduced grain boundary and electrode polarization resistances.", "These findings suggest that zinc oxide-based semiconductors and composites are attractive materials for developing new electrolyte membranes for LT-SOFCs.", "It deserves more investigation into the synthesis methods and electrochemical properties regarding the electron/ion coupling effect of the materials as well as device working principle." ]

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[ "Effect of Cation Ordering on the Performance and Chemical Stability of Layered Double Perovskite Cathodes Effect of Cation Ordering on the Performance and Chemical Stability of Layered Double Perovskite Cathodes Bernuy-LopezCarlos1*†Rioja-MonllorLaura1NakamuraTakashi2RicoteSandrine3O’HayreRyan4AmezawaKoji2EinarsrudMari-Ann1 https://orcid.org/0000-0002-2709-1219GrandeTor1 1Department of Material Science and Engineering, NTNU Norwegian University of Science and Technology, NO-7491 Trondheim, Norway; laura-rioja-monllor@ntnu.no (L.R.", "-M.); mari-ann.einarsrud@ntnu.no (M.", "-A.E.); tor.grande@ntnu.no (T.G.) 2Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, 2-1-1 Katahira Aoba-ku, Sendai 980-8577, Japan; t-naka@tagen.tohoku.ac.jp (T.N.); amezawa@tagen.tohoku.ac.jp (K.A.) 3Department of Mechanical Engineering, Colorado School of Mines, Golden, CO 80401, USA; sricote@mines.edu 4Department of Metallurgical and Materials Engineering, Colorado School of Mines, 1500 Illinois St., Golden, CO 80401, USA; rohayre@mines.edu *Correspondence: carlos.bernuy-lopez@sandvik.com; Tel.: +46-26263411 †Current address: AB Sandvik Materials and Technology, R&D, 81181 Sandviken, Sweden. 196 The effect of A-site cation ordering on the cathode performance and chemical stability of A-site cation ordered LaBaCo2O5+δ and disordered La0.5Ba0.5CoO3−δ materials are reported.", "Symmetric half-cells with a proton-conducting BaZr0.9Y0.1O3−δ electrolyte were prepared by ceramic processing, and good chemical compatibility of the materials was demonstrated.", "Both A-site ordered LaBaCo2O5+δ and A-site disordered La0.5Ba0.5CoO3−δ yield excellent cathode performance with Area Specific Resistances as low as 7.4 and 11.5 Ω·cm2 at 400 °C and 0.16 and 0.32 Ω·cm2 at 600 °C in 3% humidified synthetic air respectively.", "The oxygen vacancy concentration, electrical conductivity, basicity of cations and crystal structure were evaluated to rationalize the electrochemical performance of the two materials.", "The combination of high-basicity elements and high electrical conductivity as well as sufficient oxygen vacancy concentration explains the excellent performance of both LaBaCo2O5+δ and La0.5Ba0.5CoO3−δ materials at high temperatures.", "At lower temperatures, oxygen-deficiency in both materials is greatly reduced, leading to decreased performance despite the high basicity and electrical conductivity.", "A-site cation ordering leads to a higher oxygen vacancy concentration, which explains the better performance of LaBaCo2O5+δ.", "Finally, the more pronounced oxygen deficiency of the cation ordered polymorph and the lower chemical stability at reducing conditions were confirmed by coulometric titration. proton ceramic fuel cells (PCFC) cathode layered double perovskite 1.", "Introduction Proton ceramic fuel cells (PCFC) can potentially overcome some of the challenges currently limiting the commercial application of conventional solid oxide fuel cells (SOFCs) [1,2,3,4].", "The main difference between conventional SOFCs and PCFCs is the electrolyte material.", "While SOFCs employ oxide-ion conducting electrolytes, PCFCs make use of proton-conducting electrolytes instead.", "As the activation energy for protons is lower than for oxide ions, PCFCs can operate at lower temperatures than conventional SOFCs, i.e., 400–600 °C [5] vs. 700–900 °C.", "However, one of the main issues confronting PCFCs is the lack of high performance cathode materials [1].", "A suitable cathode material for PCFCs must facilitate the reduction of oxygen to water by reacting with protons that diffuse through the proton-conducting electrolyte.", "An ideal high-performance cathode material should combine the conduction of electrons (or holes), oxide ions and protons at the same time [6,7].", "Equally important, the material must be chemically stable at the operating conditions.", "Mixed oxide-ion- and electron-conducting materials with a perovskite structure are the most promising cathodes so far.", "Unfortunately, the best cathode materials for conventional SOFCs, such as La0.6Sr0.4Co0.2Fe0.8O3−δ (LSCF) [8] and Ba0.5Sr0.5Co0.8Fe0.2O3−δ (BSCF) [8], do not seem to present proton conductivity despite their good electronic and oxide-ion conductivities.", "Several key parameters in perovskite oxides can be tuned to enhance proton conductivity while ensuring good electronic and oxide-ion-conductivity: these include crystallographic structure, oxygen vacancy concentration, electrical conductivity and basicity [6,9,10,11].", "Regarding the crystallographic structure it is established that cubic structures favor both ionic and electronic conductivity [5].", "In respect to the oxygen vacancy concentration, high oxygen vacancy concentration can enhance proton conductivity at intermediate temperatures as a result of the Wagner hydration reaction [12,13]: H 2 O + V O • • + O O x ↔ 2 OH O • In addition, electrical conductivity above 1 S/cm is required for adequate cathode performance [3].", "Finally, high Ba content is desirable as it leads to higher oxide basicity and thereby a greater degree of protonation of the oxygen vacancies [13,14].", "Layered double perovskite materials with the general formula LnBaM2O5+δ (Ln = lanthanide or Y; M = transition metal) have been studied as potential electrodes for both PCFC [15,16,17,18] and SOFC due to their outstanding mixed electronic and oxide-ion conductivities [19,20].", "Ln and Ba occupy the A-site in this double perovskite AA′B2O6-type crystal structure, while M occupies the B-site.", "A-site cation ordering is adopted due to the large difference of size between Ba and Ln with LnO and BaO layers in dodecahedral coordination separated with MO6 layers in octahedral coordination [21].", "Cation ordering results in a decrease of symmetry.", "Layered double perovskite materials can adopt large concentrations of oxygen vacancies and depending on the size of Ln and the nature of M, the material will adopt either a tetragonal or an orthorhombic symmetry as vacancy ordering occurs [22].", "A-site cation ordering is reported to be beneficial for oxide-ion conductivity [23] while the ordering of the oxygen vacancies is detrimental [24].", "Strandbakke et al. have reported outstanding performance for the layered double perovskite La0.2Gd0.8BaCo2O5+δ [16] as a PCFC cathode with Area Specific Resistances (ASR) as low as 6 Ω·cm2 at 400 °C and 3% H2O in air.", "The large oxygen vacancy concentration adopted by the layered double perovskite seems to favor proton incorporation and sufficient proton conductivity.", "The performance is comparable to that of mixed electron/proton conducting single perovskite materials such as BaCo0.4Fe0.4Zr0.1Y0.1O3−δ (BCFZY) [3] (ASR = 10 Ω·cm2 at 400 °C in 3% humidified air), although the benefits of the layered double perovskite crystal structure are still unclear.", "LaBaCo2O5+δ represents an interesting model system to study the influence of ordering effects on the performance of PCFC cathode materials.", "In addition to the A-site ordered phase, this material can also adopt an A-site cation disordered cubic structure, represented as La0.5Ba0.5CoO3−δ, due to the larger size of La compared with other Ln elements.", "In our recent work [25], we demonstrated that the ordered LaBaCo2O5+δ phase is a metastable variant of the A-site cation disordered phase, La0.5Ba0.5CoO3−δ.", "Several authors have studied the effects of A-site cation ordering on the performance of LaBaCo2O5+δ and La0.5Ba0.5CoO3−δ for SOFC application [26,27,28], although it has yet to be studied for PCFC application.", "Both the ordered and disordered variants demonstrate low polarization resistances at temperatures as low as 600 °C (<0.2 Ω·cm2) due to the excellent mixed conducting (electron hole and oxide-ion) nature of the material.", "In addition, Garces et al. have studied the influence of the A-site cation ordering on the mixed electronic and oxide-ion conducting properties in this system [29,30].", "They obtained a noticeable improvement of performance with A-site cation ordering (0.35 Ω·cm2 for La0.5Ba0.5CoO3−δ vs. 0.12 Ω·cm2 for LaBaCo2O5+δ at 600 °C in air).", "In this work, we examine proton conducting electrolyte supported symmetric cells employing both A-site cation ordered and disordered materials (LaBaCo2O5+δ and La0.5Ba0.5CoO3−δ) to evaluate the effect of A-site cation ordering on performance for PCFC cathode applications.", "Cathode performance is evaluated by impedance spectroscopy and the results are analyzed with respect to crystal structure, basicity, oxygen content and ordering, and electrical conductivity.", "Finally, chemical compatibility between the cathode and the electrolyte is reported as well as chemical stability and oxygen deficiency by coulometric titration. 2.", "Experimental 2.1.", "Preparation of the Materials La0.5Ba0.5CoO3−δ was obtained by spray pyrolysis (Cerpotech AS, Tiller, Norway, purity > 99%) of nitrate precursors as described elsewhere [25].", "The as-sprayed powders were calcined at 1100 °C for 12 h in air in order to obtain a single pure phase.", "LaBaCo2O5+δ was obtained by calcining La0.5Ba0.5CoO3−δ in slightly lower pO2 (N2 atmosphere, pO2 ~ 10−4 atm) at 1100 °C for 12 h.", "Phase purity for all materials were determined using a Bruker D8 Advance DaVinci X-ray diffractometer (Trondheim, Norway).", "BaZr0.9Y0.1O3−δ (BZY10) powder was prepared by spray pyrolysis (Cerpotech AS, Tiller, Norway, purity > 99%) of nitrate precursors as described elsewhere [31].", "Green pellets of 20 mm diameter were prepared and sintered at 1650 °C for 10 h as described by Sazinas et al. [32].", "Prior to electrode deposition, the pellets were polished with SiC paper and washed with ethanol.", "Electrode slurries of LaBaCo2O5+δ and La0.5Ba0.5CoO3−δ were prepared by mixing 5 g of each powder with 1 g dispersant (20 wt % solsperse 28,000 (Lubrizol, Wickliffe, OH, USA) dissolved in terpineol), and 0.3 g binder (5 wt % V-006 (Heraeus, Hanau, Germany) dissolved in terpineol).", "Electrolyte-supported symmetric cells for LaBaCo2O5+δ and La0.5Ba0.5CoO3−δ were produced by screen painting the corresponding slurries on both sides of a dense BZY10 pellet (geometrical density >90%).", "The thickness of the BZY10 electrolyte was about 800 μm after polishing and electrode thicknesses were ~20–25 μm.", "Thickness was checked by scanning electron microscopy (SEM).", "SEM images were captured on a field emission gun SEM (Zeiss Ultra 55, Limited Edition, Oberkochen, Germany).", "The symmetric cells of both LaBaCo2O5+δ and La0.5Ba0.5CoO3−δ materials were fired at 600 °C for 2 h in ambient air to form porous cathode layers.", "Gold paste (Fuel Cell Materials) was applied onto the cathodes for current collection followed by in-situ curing.", "Pt wires were employed as conducting wires. 2.2.", "Electrochemical Characterization Symmetric cells were characterized by electrochemical impedance spectroscopy (EIS) in dry and moist (pH2O = 0.03 atm) synthetic air and N2 from 600 to 400 °C, at temperature intervals of 50 °C (with a cooling rate of 1 °C/min and 8 h dwell before each measurement) using a ProboStatTM (NorECs AS, Oslo, Norway) set-up and an Alpha A (Novocontrol Technologies, Montabaur, Germany) impedance analyzer.", "The signal amplitude was 50 mV under open circuit voltage (OCV) in the 10−2–106 Hz frequency range.", "The 3% humidification was achieved by bubbling the gases through distilled water at 25 °C.", "The equivalent circuit fitting and analysis of the impedance data were carried out using Zview Software v3.5. 2.3.", "Oxygen Deficiency and Chemical Stability Compatibility tests between the electrode and the electrolyte materials were performed by mixing together about 1 g each of both materials in an agar mortar for 15 min.", "Pellets of 15 mm diameter were fabricated and exposed to different thermal treatments: 1000 °C, 1100 °C and 1200 °C for 72 h at each temperature.", "High Temperature X-ray diffraction (HT-XRD) measurements were performed using a Bruker D8 Advance diffractometer equipped with an MRI TCP20 high temperature camera (Sendai, Japan).", "A Pt strip-type resistive heater functioned as the sample support.", "XRD patterns (20–85°, about 30 min collection time) were recorded from 600 to 1200 °C in air, at 100 °C intervals.", "An S-type thermocouple was used for temperature determination using the radiant heater.", "The heating rate and dwell time before data collection were 0.1 °C/s and 10 min respectively Finally, coulometric titration of both LaBaCo2O5+δ and La0.5Ba0.5CoO3−δ materials was performed to determine the oxygen content and the chemical stability of these materials below 10−4 bar.", "The details of the experiment and the set-up are given elsewhere [33,34]. 3.", "Results 3.1.", "Microstructure of the Symmetric Cells X-ray diffraction of the two materials, as reported in our previous work [25], established the phase purity and crystal structure: cubic for La0.5Ba0.5CoO3−δ and tetragonal for LaBaCo2O5+δ.", "Figure 1 provides representative low and high-magnification SEM images of a La0.5Ba0.5CoO3−δ symmetric cell.", "Despite the low preparation temperature of the symmetric cells, sufficient adherence to the electrolyte was obtained.", "Higher processing temperatures lead to delamination and poor adherence of the electrolyte.", "Electrode thickness of about 20 μm and average grain size below ~1 μm are observed.", "LaBaCo2O5+δ shows similar microstructure as shown in Figure S1. 3.2.", "Electrochemical Performance Figure 2 depicts typical Nyquist plots obtained for symmetric cells of the A-site cation disordered La0.5Ba0.5CoO3−δ and A-site cation ordered LaBaCo2O5+δ materials in moist synthetic air at 500 °C.", "Both A-site cation disordered and ordered materials present similar Nyquist plots for all temperatures as illustrated in Figure 2.", "Two main contributions coming from the electrolyte and the electrode are observed.", "The equivalent circuit model used to fit the data is LR (RQ)(RQ)(RQ), where L, R and Q are inductance, resistance and constant phase element respectively.", "The resistor (RBZY10_1) and the first RQ element (RBZY10_2 and CPEBZY10_2, blue semicircle) are assigned to the electrolyte of the symmetric cells.", "The two other RQ elements (i.e., RSP_1, CPESP_1, RSP_2, CPESP_2, green and violet semicircles respectively for La0.5Ba0.5CoO3−δ) correspond to the electrode response of the cells.", "The assignment of these electrochemical processes was carried out by evaluating the pseudocapacitance of the RQ elements (Table S1 for both La0.5Ba0.5CoO3−δ and LaBaCo2O5+δ) obtained with the electrochemical model: i.e., La0.5Ba0.5CoO3−δ; ~10−10 F/cm2 for the first RQ element, assigned as the response of the electrolyte [8,9,10,35,36,37,38,39,40,41]; ~10−4 F/cm2 and 10−2 F/cm2 for the other two RQ elements, assigned as the response of the electrode [8,9,10,35,36,37,38,39,40,41].", "Total cathode Area Specific Resistances (ASRs) were obtained by dividing the sum of the electrode resistances (i.e., RSP_1 and RSP_2 in Figure 2 for La0.5Ba0.5CoO3−δ) by two.", "Division by a factor of two accounts for the fact that the combined contribution from two cathode electrode responses are measured in symmetric cell testing.", "Resulting cathode ASR values of both LaBaCo2O5+δ and La0.5Ba0.5CoO3−δ materials are shown in Figure 3 in 3% moist synthetic air.", "Both LaBaCo2O5+δ and La0.5Ba0.5CoO3−δ materials exhibit excellent performance in the temperature range 400–600 °C.", "Despite the similar microstructure of both materials, the A-site cation ordered material LaBaCo2O5+δ gives a better performance than the A-site disordered La0.5Ba0.5CoO3−δ material.", "Cathode ASR values for LaBaCo2O5+δ at 600 and 400 °C are 0.15 and 7.4 Ω·cm2, respectively.", "The corresponding values for La0.5Ba0.5CoO3−δ at 600 and 400 °C are 0.32 and 11.5 Ω·cm2, respectively.", "Activation energies are also given in Figure 3 for both La0.5Ba0.5CoO3−δ and LaBaCo2O5+δ materials, with higher Ea for A-site cation ordered LaBaCo2O5+δ.", "For each material, the total electrode response can be deconvoluted in two main processes: an intermediate/middle frequency (RSP_1CPESP_1) process and a low frequency process (RSP_2CPESP_2).", "The intermediate frequency (MF) process exhibits lower pseudocapacitances than the low frequency (LF) process (~10−4 F/cm2 vs. 10−2 F/cm2).", "The deconvolution of the electrochemical data for both LaBaCo2O5+δ and La0.5Ba0.5CoO3−δ materials is shown in Figure 4.", "Similar trends are observed for both materials: below 550 °C, the LF process appears to be rate limiting, while the MF process becomes limiting at higher temperatures.", "Further investigation, e.g., pO2- and pH2O-dependent experiments would be needed to further assign these MF and LF processes to specific electrochemical reactions taking place in the electrode [39].", "Figure 5 shows the Nyquist plots for La0.5Ba0.5CoO3−δ in N2 atmosphere at 500 °C in dry (Figure 5a) and moist conditions (Figure 5b).", "ASR values for the electrode contribution extracted from these data are represented in Figure 6.", "It is found that the ASR decreases in N2 when the atmosphere is humidified.", "It can also be observed that A-site cation ordering does not give any improvement in the ASR as both A-site cation ordered and disordered materials lead to the same performance in moist conditions at low pO2. 3.3.", "Chemical Stability The chemical potential of oxygen and stability of the two polymorphs in reducing conditions were investigated by coulometric titration and the results are shown in Figure 7.", "The oxygen deficiency increases with decreasing oxygen partial pressure as expected, but the slope is significantly different for the two polymorphs.", "The difference in slope demonstrates the superior stability of Co in a higher oxidation state in La0.5Ba0.5CoO3−δ relative to LaBaCo2O5+δ.", "This is further confirmed by the onset of decomposition (vertical relationship of stoichiometry versus pO2) of LaBaCo2O5+δ at a higher pO2 relative to La0.5Ba0.5CoO3−δ at constant temperature.", "Moreover, the coulometric data also proves that the cation-ordered phase tolerates a higher oxygen deficiency before decomposition although this could be an effect of the kinetics of the decomposition reaction.", "The thermal stability of LaBaCo2O5+δ in air was studied by high temperature X-ray diffraction and the diffraction patterns are shown in Figure 8.", "Only thermal expansion of LaBaCo2O5+δ was observed up to 1100 °C.", "These data are consistent with our previous study [25] where LaBaCo2O5+δ was shown to remain tetragonal at high temperature with a P4/mmm as space group.", "This means that the material remains A-site ordered at the studied temperature range (RT-800 °C).", "However, Figure 8 shows that LaBaCo2O5+δ starts to transform into La0.5Ba0.5CoO3−δ at 1100 °C, with complete disappearance of the splitting of the Bragg reflections due to the loss of A-site cation ordering at 1200 °C (Figure 8b).", "This means that there is a phase transition from tetragonal P4/mmm structure of LaBaCo2O5+δ to cubic P 3 ̄ m m m structure of La0.5Ba0.5CoO3−δ close to 1100 °C in air.", "Finally, a good compatibility between both LaBaCo2O5+δ and La0.5Ba0.5CoO3−δ materials and BZY10 electrolyte material is demonstrated by X-ray diffraction of powder mixtures annealed at different temperatures (Figure S2).", "Temperatures close to 1200 °C for 72 h are required to initiate (minor) secondary phase formation in a powder mixture of the two materials with the electrolyte.", "Both PCFC operation temperatures (400–600 °C) and electrode sintering temperature (600 °C) are well below the temperature where cathode/electrolyte reactions are observed to initiate. 4.", "Discussion 4.1.", "Comparison with Literature Figure 9 compares the performance of both LaBaCo2O5+δ and La0.5Ba0.5CoO3−δ materials with the two best PCFC cathode materials reported in the literature: the single perovskite BaCo0.4Fe0.4Zr0.1Y0.1O3−δ (BCFZY) [3] and the layered double perovskite La0.2Gd0.8BaCo2O5+δ (LGBC) [16].", "The comparison is carried out by taking literature data measured in the same configuration (four-electrode measurements of electrolyte supported symmetric cells), rather than complete fuel cells.", "One well known issue with symmetric cell measurements involving PCFC electrolytes in oxidizing atmospheres is the influence of the parasitic p-type conductivity of the electrolyte itself [16] on the apparent measured cathode ASR (especially at high temperatures) [42].", "This parasitic p-type electronic conductivity leads to an overestimation of the performance of the electrode and makes the interpretation of the data more complex.", "Thus, it is not recommended to compare cathode ASR results obtained from complete fuel cells to the results obtained from symmetric cell studies.", "Symmetric cell comparisons, however, are likely to be reasonable if the investigations employ similar electrolyte compositions and thicknesses.", "Based on such symmetric cell comparisons, the performance of both LaBaCo2O5+δ and La0.5Ba0.5CoO3−δ materials are comparable to LGBC and BCFZY, with even better performance at temperatures above 500 °C.", "These comparisons underscore the high potential of both LaBaCo2O5+δ and La0.5Ba0.5CoO3−δ materials as PCFC cathodes.", "Activation energies are summarized in Figure 9.", "Both LaBaCo2O5+δ and La0.5Ba0.5CoO3−δ materials have higher activation energies than LGBC and BCFZY, which suggests differences in the electrode electrochemical mechanism.", "A preliminary assignment of the electrochemical mechanism can be suggested by looking at the temperature dependence of the deconvoluted electrochemical processes shown in Figure 4.", "The low frequency process is hardly dependent on the temperature which may be assigned to the oxygen adsorption/dissociation processes at all, while the intermediate frequency process may be assigned to charge transfer processes due to the higher temperature dependency of this process.", "This is consistent with previous works in the literature on materials with similar perovskite structure [16,38].", "In addition to this, it is well-known that the microstructure of cathode materials plays a crucial role for the electrochemical properties.", "Adler et al. [43] published a detailed study on the electrode kinetics of porous mixed-conducting oxygen electrodes based on oxide-ion conducting electrolyte, using a continuum modeling to analyze the oxygen reduction reaction.", "Furthermore, Strandbakke et al. [44] showed that pre-exponential values of the Arrhenius plot are indicative of the microstructure impact in the electrochemical performance.", "A similar microstructure for both LaBaCo2O5+δ and La0.5Ba0.5CoO3−δ materials can be seen in Figure S1 and can also be confirmed with the similar pre-exponential values calculated from Figure 9 (13.55 for La0.5Ba0.5CoO3−δ and 14.75 for LaBaCo2O5+δ).", "However, experiments at different pO2 and pH2O and more detailed microstructure studies (determination of the tortuosity, surface area, etc.) are necessary to successfully assign the electrochemical processes and to correlate them with the electrode microstructure [39].", "Table 1 summarizes the structure, Ba content, performance, oxygen content and electrical conductivities of LaBaCo2O5+δ and La0.5Ba0.5CoO3−δ.", "The table also includes data for BCFZY [3,13] and LGBC [16,43].", "Therefore, due to the similar microstructure discussed previously we attempt a correlation between all these parameters to help rationalize the performance differences between these various cathode materials. 4.2.", "Correlation between ASR, Electrical Conductivity, Basicity and Oxygen Content The ASR and the oxygen content as a function of temperature for both La0.5Ba0.5CoO3−δ and LaBaCo2O5+δ materials are shown in Figure 10a.", "Likewise, the ASR and the electrical conductivity vs. temperature are plotted in Figure 10b.", "Data for the single perovskite BCFZY [3,13] and the layered double perovskite LGBC [16,45] materials extracted from the literature are added for comparison.", "Two observations are evident from these two figures: (1) a lower oxygen deficiency of La0.5Ba0.5CoO3−δ and LaBaCo2O5+δ compared to BCFZY and LGBC; (2) a significantly lower (nearly two orders of magnitude) electrical conductivity for BCFZY.", "The lower performance of La0.5Ba0.5CoO3−δ in comparison to LaBaCo2O5+δ at lower temperatures can be explained by the lower oxygen vacancy concentration in La0.5Ba0.5CoO3−δ as shown in Figure 10.", "The enhanced low-temperature oxygen vacancy concentrations for both LGBC and BCFZY materials appear to be consistent with their higher low-temperature cathode performance.", "Protonation of oxygen vacancies generally increases with oxide basicity [13,14].", "All else being equal, it is therefore expected that more basic materials will have higher performance levels as PCFC cathodes.", "In addition, higher oxygen vacancy concentration should drive higher protonation according to Le Chatelier’s principle.", "Zohourian et al. [13] and Strandbakke et al. [16] have measured the hydration level in BCFZY and LGBC.", "Despite their high level of oxygen vacancies both materials are only able to hydrolyze 1% of the available oxygen vacancies at 400 °C.", "Because of its higher basicity, a greater fraction of vacancies is expected to be hydrolyzed in BCFZY.", "Nevertheless, Figure 9 and Table 1 show that at 400 °C the performance of the layered double perovskite material is better than the materials with single perovskite structure.", "One possible explanation of this difference could be that A-site cation ordering enhances protonation due to the different local environments of the oxygen vacancies in the two crystal structures.", "The similar performance of LaBaCo2O5+δ and LGBC can also be explained by the higher basicity of the A-site cations in LaBaCo2O5+δ.", "A-site cation ordering in LaBaCo2O5+δ leads to higher performance [30] due to the higher oxygen vacancy concentration as shown in Figure 10a.", "The higher oxygen vacancy concentration and therefore higher degree of protonation could rationalize the higher performance of LaBaCo2O5+δ compared to La0.5Ba0.5CoO3−δ Furthermore, both LaBaCo2O5+δ and La0.5Ba0.5CoO3−δ as well as BCFZY have been shown to be very good oxide ion conductors [26,27,28,46].", "Therefore, the main difference in performance between BCFZY and both LaBaCo2O5+δ and La0.5Ba0.5CoO3−δ materials may arise from the differences in electrical conductivity as shown in Figure 10b in addition to a difference in proton conductivity.", "Measurements in low pO2 conditions have been proposed in order to eliminate the presence of oxide-ions and isolate the proton conduction contribution when examining prospective PCFC cathodes [16].", "As shown in Figure 5, a decrease in ASR and Ea for both LaBaCo2O5+δ and La0.5Ba0.5CoO3−δ is observed in humidified inert atmosphere (pO2 = 10−4 atm).", "This decrease may suggest the presence of proton conductivity in the material, and is similar to what was observed for LGBC by Strandbakke et al. [16]. 4.3.", "Chemical Stability of the Two Polymorphs Previous studies of the oxygen non-stoichiometry of the two polymorphs have suggested that La0.5Ba0.5CoO3−δ is the most stable polymorph at oxidation conditions and low temperature [25].", "The coulometric titration data (Figure 7) confirms that the oxygen content of LaBaCo2O5+δ is lower than La0.5Ba0.5CoO3−δ independent of temperature and oxygen partial pressure.", "The lower oxygen partial pressure at the decomposition suggests that La0.5Ba0.5CoO3−δ is more stable than LaBaCo2O5+δ also under reducing conditions.", "It has previously been shown that La0.5Ba0.5CoO3−δ can be transformed to LaBaCo2O5+δ by annealing in N2 at 1100 °C [25], while we demonstrated in this work that the transverse phase transition is observed in air close to 1100 °C.", "Based on these two observations LaBaCo2O5+δ is the stable polymorph at inert conditions and LaBaCo2O5+δ the most stable in air close to 1100 °C.", "Evidence for a phase transition between the two polymorphs could not be obtained by coulometric titration up to 800 °C (Figure 7).", "The phase transition is however reconstructive in nature and only occurs above a critical temperature for sufficient cation mobility.", "It is therefore likely that true equilibrium between the two phases could not be obtained during the coulometric titration before decomposition.", "Additional measurements are therefore required to determine accurately the relative stability of the two polymorphs and the T-pO2 dependence of the phase transition between the two polymorphs. 5.", "Conclusions LaBaCo2O5+δ and La0.5Ba0.5CoO3−δ materials have been tested as cathodes for protonic ceramic fuel cells and both exhibit good stabilities.", "The A-site cation ordered LaBaCo2O5+δ material possesses better performance than the A-site cation disordered La0.5Ba0.5CoO3−δ materials with ASR values as low as 7.4 and 0.16 Ω·cm2 at 400 and 600 °C respectively.", "Both LaBaCo2O5+δ and La0.5Ba0.5CoO3−δ demonstrate competitive performance with the best state-of-the-art cathode materials BaCo0.4Fe0.4Zr0.1Y0.1O3−δ and La0.2Gd0.8BaCo2O5+δ.", "Oxygen vacancy concentration, electrical conductivity, crystal structure and basicity are shown to be key, interconnected parameters that govern PCFC cathode performance.", "The A-site cation ordered LaBaCo2O5+δ material exhibits better performance at low temperature than the A-site cation disordered La0.5Ba0.5CoO3−δ material because it retains higher oxygen vacancy concentration at low temperatures.", "In addition, A-site cation ordering is hypothesized to increase the basicity of the oxygen vacancies, making them more likely to hydrate.", "The similar low-temperature performance of A-site cation ordered LaBaCo2O5+δ material vs.", "La0.2Gd0.8BaCo2O5+δ (LGBC) may be explained by an increase of the basicity in LaBaCo2O5+δ.", "As the temperature increases, the A-site cation ordered LaBaCo2O5+δ material shows better relative performance compared to the A-site cation disordered La0.5Ba0.5CoO3−δ due to the increase in oxygen vacancy concentration.", "This work shows the importance of understanding and controlling crystal structure, basicity, oxygen vacancy concentration and electrical conductivity in order to improve PCFC cathode materials while keeping an eye on the chemical stability of the material." ]

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[ "Novel Composite Electrolytes of Zr0.92Y0.08O2-α(8YSZ)-Low Melting Point Glass Powder for Intermediate Temperature Solid Oxide Fuel Cells Novel Composite Electrolytes of Zr0.92Y0.08O2-α(8YSZ)-Low Melting Point Glass Powder for Intermediate Temperature Solid Oxide Fuel Cells https://orcid.org/0000-0002-2482-6320WangHongtao*DuRuifengShiRuijuanLiuJunlong School of Chemical and Material Engineering, Fuyang Normal College, Anhui Provincial Key Laboratory for Degradation and Monitoring of Pollution of the Environment, Fuyang 236037, China; ruifengdu1@163.com (R.D.); rjshi@fync.edu.cn (R.S.); jlliu@fync.edu.cn (J.L.)", "*Correspondence: hongtaoking3@163.com; Tel.: +86-558-2596-249; Fax: +86-558-2596-703 1221 In this study, Zr0.92Y0.08O2-α(8YSZ) powders were synthesized by the sol-gel method.", "The chemical physics changes and phase formation temperature of 8YSZ crystal were determined by thermogravimetry analysis and differential scanning calorimetry (TGA-DSC). 8YSZ-low melting point glass powder (8YSZ-glass) composite electrolytes with various weight ratios were prepared and calcined at different temperatures.", "The X-ray diffraction (XRD) patterns of the composite electrolytes were tested.", "The effects of synthesis temperature, weight ratio, test temperature, and oxygen partial pressure on the conductivities of 8YSZ-glass composite electrolytes, were also investigated at 400–800 °C.", "The result of the logσ ~ log(pO2) plot indicates that the 8YSZ-20% glass (700 °C) is almost a pure ionic conductor.", "The oxygen concentration discharge cell illustrates that the 8YSZ-20% glass (700 °C) composite electrolyte is a good oxygen ion conductor. defects electrolyte fuel cell ceramics sol-gel preparation 1.", "Introduction ZrO2-based electrolytes doped, with rare earth metallic cations, are excellent oxide ionic conductors, and they are widely used in oxygen sensors and solid oxide fuel cells (SOFCs) [1,2,3,4] due to their good mechanical strength and high ionic transport numbers.", "During the past decades, continuous research concentrating on Y2O3-stabilized ZrO2 (YSZ) has been done [5,6].", "For example, Caruso et al. investigated the influence of different parameters on the morphology and microstructure of YSZ powders synthesized by the sol-gel method [5].", "However, SOFCs using YSZ as electrolyte membrane usually run at high temperatures (800–1000 °C).", "Therefore, researchers have focused on two ways to lower the operating temperature of YSZ.", "One strategy is to use YSZ films, and the other way is to construct composite electrolytes, which may have the combined advantages of each component [7,8,9,10,11].", "A few research reports have shown that the thin film fuel cells using YSZ as membrane electrolytes generated maximum power output densities of 200–400 mW·cm−2 at 800 °C [12,13,14].", "Singh et al. reported that the YSZ-SDC (samarium doped ceria) composite electrolyte with a weight ratio 8.5:1.5 has a higher electrical conductivity than single material YSZ at 400–700 °C [9].", "It is well known that silicate, borate, mica, and other glass systems are commonly used as sealing materials in fuel cell systems [15,16,17,18].", "It may be expected that using silicate low melting point glass powder, as a sintering aid, as well as composite electrolytes with improved gas tightness, durability, and better component matching, could be synthesized.", "In this study, novel composite electrolytes of Zr0.92Y0.08O2-α(8YSZ)-low melting point glass powder were synthesized.", "The morphology, structure, and intermediate temperature electrochemical properties of the composite electrolytes were investigated by a variety of methods. 2.", "Experimental We initially synthesized Zr0.92Y0.08O2-α(8YSZ) electrolyte via a sol-gel method using citric acid as a chelating agent as reported previously [19].", "All the reagents used are analytical-grade.", "Firstly, Y2O3 was dissolved in nitric acid and Zr(NO3)4·5H2O was dispersed into distilled water.", "The solution was then mixed with citric acid and NH4OH and evaporated at 90 °C to get a gel.", "After gelation and ashing treatment, the obtained ash was calcined at 700 °C, 1200 °C and 1550 °C for 6 h, respectively, to get Zr0.92Y0.08O2-α(8YSZ) powder.", "The low melting point glass powder was used as a sintering aid to form composite.", "The composition of the low melting point glass powder is Na2O-CaO-SiO2-ZnO (Taizhou Xinhai Special Materials Factory, 300 mesh, m.p. is 550 °C). 8YSZ and low melting point glass powder were mixed with a weight ratio of four to one and heated at 700 °C, 1200 °C and 1550 °C for 2 h, correspondingly.", "The composites with weight ratio of 8YSZ: low melting point glass powder = 9:1 and 7:3 were also synthesized at 700 °C.", "These results are summarized in Table 1.", "The chemical physics changes and phase formation temperature of 8YSZ crystal were determined by thermogravimetry analysis and differential scanning calorimetry (TGA-DSC) (TGA-DSC, Universal V 3.7A, TA Instruments, New Castle, DE, USA).", "The X–ray diffraction (XRD) (XRD, X’pert Pro MPD, Amsterdam, Netherlands)patterns of the above electrolytes were tested with a Panalytical X′Pert Pro MPD diffractometer.", "The morphology of the 8YSZ-20% glass (700 °C) was observed using a scanning electron microscope (SEM, S-4700, Hitachi, Tokyo, Japan) [20,21].", "The conductivities vs. different synthesis temperature, test temperature, oxygen partial pressure and weight ratio in nitrogen atmosphere were tested with an electrochemical analyzer (CHI660E, Shanghai, China) at 400–800 °C.", "All the samples were ground into thin slices of 1.0–1.2 mm.", "A 20% palladium-80% silver paste with silver wires was used to fabricate the electrodes (area: 0.5 cm2).", "Oxygen concentration discharge fuel cell and H2/O2 fuel cell using the 8YSZ-20% glass (700 °C) as electrolyte were constructed [22,23]. 3.", "Results and Discussion The TGA and DSC curves of the Zr0.92Y0.08O2-α(8YSZ) gel heated at 15 °C·min−1 in nitrogen atmosphere up to 1000 °C are shown in Figure 1.", "It can be seen that the TGA curve shows a weight loss about 7% from 35 °C to 130 °C corresponding to two weak endothermic peaks in DSC curve, which is attributed to the residual water in the 8YSZ gel [24,25].", "About seventy percent of weight loss of 8YSZ gel occurred up to c.a. 500 °C.", "The first calcined temperature was fixed at 700 °C because there is almost no weight loss at 520 °C and above [26,27].", "The XRD patterns of 8YSZ and 8YSZ-glass obtained with different weight ratio and calcined at different synthesis temperature are shown in Figure 2.", "Figure 2a shows the XRD patterns of the 8YSZ-glass with different weight ratio calcined at 700 °C, i.e., 0%, 10%, 20% and 30%.", "All the samples possess coexisting tetragonal and monoclinic phases, where tetragonal is the major phase.", "The XRD angles at 30.14°, 34.72° and 35.04° belong to the (101), (002), and (110) crystal planes of t-Zr0.9Y0.1O1.95 (JCPDS 82-1241), respectively.", "From Figure 2b, when the synthesis temperature reaches 1200 °C and 1550 °C, the XRD patterns of 8YSZ are merely tetragonal structures.", "However, there are still a few obvious diffraction peaks of monoclinic structure in 8YSZ-20% glass calcined at 1200 °C and 1550 °C, respectively.", "Mori et al. observed that the Ti4+-doped 8YSZ electrolyte transform from a pure cubic structure to two-phase compound containing small amount of tetragonal phase with increasing Ti content [28].", "And a monoclinic-to-tetragonal phase transformation was found in 9 mol% MgO doped ZrO2 above 1300 °C [29].", "Therefore, it is probably the high synthesis temperature and 20% weight ratio of low melting point glass leads to the appearance of monoclinic phase.", "Besides, a diffraction peak is observed at 2θ ≈ 26° may be indexed to the SiO2 (JCPDS 13-0026) or Na2Si3O7 (JCPDS 38-0019).", "This indicates that the Na2O-SiO2 in low melting point glass changes from amorphous to crystalline at high temperature.", "The conductivities vs. different synthesis temperature and weight ratio were tested at 400–800 °C in nitrogen atmosphere as shown in Figure 3.", "It is clear that the conductivities of composite electrolytes increase with the increase in glass concentration.", "And the highest conductivities are obtained for the 8YSZ-20% glass (700 °C), 8YSZ-20% glass (1200 °C), and 8YSZ-20% glass (1550 °C) to be 5.7 × 10−2 S·cm−1, 4.1 × 10−3 S·cm−1, and 2.3 × 10−2 S·cm−1 at 800 °C, respectively.", "A recent investigation by Lee et al. [29] reported that a single cubic phase of 8YSZ showed higher conductivity than 9 mol% MgO doped ZrO2 which has a mixed phase.", "Similarly, the conductivities of the 8YSZ-20% glass (700 °C) (Figure 3a) and 8YSZ-20% glass (1550 °C) (Figure 3b) are higher than that of 8YSZ-20% glass (1200 °C) (Figure 3b) which has evidently tetragonal and monoclinic biphasic structure in Figure 2b.", "The conductivities of the 8YSZ-20% glass (700 °C) are lower than that of 8YSZ-30% glass (700 °C) composite electrolyte as shown in Figure 3a.", "However, the 8YSZ-30% glass (700 °C) composite electrolyte is unstable because it will cause segregation and reduce the mechanical hardness in the molten state when the glass powder is too high in percentage.", "Figure 4 shows the variation of conductivity of 8YSZ-30% glass (700 °C) composite electrolyte with time in nitrogen atmosphere at 800 °C.", "The conductivity reaches a steady state in the first hour.", "However, with increasing time, the conductivity of 8YSZ-30% glass (700 °C) composite electrolyte gradually decreased.", "This suggests that it cannot be used for long period at 800 °C.", "The external (a) and cross-sectional (b) surface SEM images of the 8YSZ-20% glass (700 °C) composite electrolyte are displayed in Figure 5.", "The 8YSZ agglomerated with low melting point glass powder, few pores are observed and the microstructure is homogeneous after heating at 700 °C, which is attributed to high fluidity of molten glass.", "Figure 5 shows that the two components are evenly dispersed and intimately connected and do not react with each other due to their high chemical stability [3,5,9,11].", "In order to investigate ionic conduction of the 8YSZ-20% glass (700 °C), the relationship between the oxygen partial pressure (pO2) and conductivities was studied.", "As shown in Figure 6, there is almost a straight line within the whole pO2 range.", "The result indicates that the 8YSZ-20% glass (700 °C) is almost a pure ionic conductor [20,21,22,23].", "In the pO2 range of 10−20~10−15 atm, the curve is slightly upwarped, indicating that there is a trace electron conduction in the 8YSZ-20% glass (700 °C) in reducing atmosphere.", "It is well known that ZrO2-based electrolyte is a good oxygen ion conductor.", "To study the oxide ionic conduction of the 8YSZ-20% glass (700 °C) composite electrolyte, an oxygen concentration discharge cell was tested at 800 °C as shown in Figure 7.", "The calculational electromotive forces (EMFcal) could be obtained from EMFcal = R T 4 F tO ln[pO2 (A)/pO2 (B)] when tO = 1.", "The air (pO2 (B)) and pure O2 (pO2 (A)) are introduced into the anode and cathode, correspondingly.", "From Figure 7, the open circuit voltage is 35.6 mV, which is close to the calculated EMF (36.1 mV).", "Moreover, a stable discharge line could be seen in Figure 7.", "All the results illustrate that the 8YSZ-20% glass (700 °C) composite electrolyte is a good oxygen ion conductor.", "The H2/O2 fuel cell electrochemical performance was tested at 800 °C for the 8YSZ-20% glass (700 °C) as shown in Figure 8.", "It can be seen that the 8YSZ-20% glass (700 °C) reveals a high open circuit voltage (1.09 V) which means the composite electrolyte is dense [5].", "The maximum power density of the 8YSZ-20% glass (700 °C) is 72.7 mW·cm−2 (thickness = 1.1 mm) at 800 °C.", "The result is lower than that previous reported cathode supported thin film fuel cell with 200–400 mW·cm−2 at 800–850 °C [12,13,14,30], which can be attributed to the electrolyte thickness and the electrode/electrolyte interface.", "Further work is in progress to optimize the composition of composite electrolytes and develop the stable and high performance solid oxide fuel cell [31,32]. 4.", "Conclusions In this study, low melting point glass powder was chosen as a sintering aid to prepare novel Zr0.92Y0.08O2-α(8YSZ)-low melting point glass composite electrolytes.", "The results of XRD indicate that the major phase in composite electrolytes is tetragonal and no diffraction peaks of low melting point glass are found.", "The influences of amount of additive, synthesis temperature, test temperature, and oxygen partial pressure on the electrical conductivities of the composite electrolytes were investigated at 400–800 °C.", "The results of the XRD and conductivities show that the 8YSZ-20% glass (700 °C) is a suitable choice.", "The oxygen concentration discharge cell illustrates that the 8YSZ-20% glass (700 °C) composite electrolyte is a good oxygen ion conductor.", "The maximum power density of the 8YSZ-20% glass (700 °C) is 72.7 mW·cm−2 (thickness = 1.1 mm) at 800 °C." ]

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[ "In Situ Impedance Analysis of Oxygen Exchange on Growing\nLa0.6Sr0.4CoO3−δ Thin\nFilms In Situ Impedance Analysis of Oxygen Exchange on Growing La0.6Sr0.4CoO3−δ Thin Films RuppGhislain M.", "*KubicekMarkusOpitzAlexander K.FleigJürgen Institute of Chemical Technologies and Analytics, Vienna University of Technology, Getreidemarkt 9, Vienna, AT-1060, Austria *E-mail: ghislain.rupp@tuwien.ac.at.", "The further development of solid oxide fuel and electrolysis cells (SOFC/SOEC) strongly relies on research activities dealing with electrode materials.", "Recent studies showed that under operating conditions many perovskite-type oxide electrodes are prone to changes of their surface composition, leading to severe changes of their electrochemical performance.", "This results in a large scatter of data in literature and complicates comparison of materials.", "Moreover, little information is available on the potentially excellent properties of surfaces immediately after preparation, that is, before any degradation by exposure to other gas compositions or temperature changes.", "Here, we introduce in situ impedance spectroscopy during pulsed laser deposition (IPLD) as a new method for electrochemical analysis of mixed ionic and electronic conducting (MIEC) thin films during growth.", "First, this approach can truly reveal the properties of as-prepared MIEC electrode materials, since it avoids any alterations of their surface between preparation and investigation.", "Second, the measurements during growth give information on the thickness dependence of film properties.", "This technique is applied to La0.6Sr0.4CoO3−δ (LSC), one of the most promising SOFC/SOEC oxygen electrode material.", "From the earliest stages of LSC film deposition on yttria-stabilized zirconia (YSZ) to a fully grown thin film of 100 nm thickness, data are gained on the oxygen exchange kinetics and the defect chemistry of LSC.", "A remarkable reproducibility is found in repeated film growth experiments, not only for the bulk related chemical capacitance but also for the surface related polarization resistance (±10%).", "Polarization resistances of as-prepared LSC films are extraordinarily low (2.0 Ω cm2 in 40 μbar O2 at 600 °C).", "LSC films on YSZ and on La0.95Sr0.05Ga0.95Mg0.05O3−δ (LSGM) single crystals exhibit significantly different electrochemical properties, possibly associated with the tensile strain of LSC on LSGM. impedance PLD fuel cell SOFC electrode oxygen exchange LSC strain document-id-old-9 ae8b00586 document-id-new-14 ae-2018-005868 ccc-price Solid oxide fuel cells (SOFCs) and solid oxide electrolysis cells (SOECs) may become important technologies to ease the transition from fossil fuels to renewable resources such as biomass and hydrogen.1−4 Current applications include combined heating and power (CHP) systems, as well as auxiliary power units and typically operate at 700–900 °C.5,6 The high operating temperatures restrict the choice of materials used, complicate production, decrease the durability of the components because of undesired side reactions, and therefore hamper a broad commercialization.7 However, these challenging conditions are required for achieving sufficiently fast reaction kinetics for the oxygen incorporation or evolution at the air electrode, since reaction rates for given overpotential strongly depend on temperature (with typical activation energies in the range of 1.3–1.8 eV).8 Hence, mixed ionic and electronic conducting (MIEC) oxides are vastly investigated in order to find, understand and design materials that offer a high catalytic activity for the oxygen exchange as well as high ionic and electronic conductivity.9 For SOFCs and SOECs, porous MIEC electrodes are prepared by tape casting, screen printing or dip coating to achieve electrodes with large surface area for oxygen reduction.", "In fundamental research, however, MIEC oxides are often prepared using pulsed laser deposition (PLD) to obtain thin films with a well-defined surface, which eases systematic studies and comparison of their catalytic activity.", "Thereby, different perovskite-type oxides, such as Ba1–xSrxCo1–yFeyO3−δ (BSCF),10−12 La0.6Ba0.4CoO3−δ (LBC),13 La0.6Sr0.4CoO3−δ (LSC),13 La1–xSrxCo1–yFeyO3−δ (LSCF),8,14 La0.6Sr0.4FeO3−δ (LSF),15 Sm1–xSrxCoO3−δ (SSC),8 SrFeO3−δ (SFO),16 and SrTi1–yFeyO3−δ (STF),16 have been investigated as promising cathode candidates for SOFCs.", "An electrode material of particular interest is LSC, since it shows very high electronic conductivity (∼1000 S/cm) together with low polarization resistance for the oxygen exchange reaction (one of the lowest oxygen exchange resistances reported so far was ∼0.5 Ω cm2 for a thin film at 600 °C and 0.21 bar oxygen partial pressure13).", "Still, LSC has yet not met all stability requirements, which not only impedes commercial application but also hampers comparability of research studies.", "Severe degradation of thin film electrodes, mostly related to composition changes of the thin film surface, may occur on the time scale of hours or even faster and affects reproducibility of data.17−20 A recent study revealed that LSC surfaces might be very inhomogeneous in terms of their oxygen exchange current density, with only a few highly active, presumably Co related reaction sites in an otherwise less active Sr-terminated surface environment.19,21 It was shown that minor surface composition changes, hardly detectable by analytical methods, had a significant impact on the oxygen exchange kinetics.", "These insights were gained by a novel method, which allows manipulation of the electrode surface and in situ measurement of the impedance inside a PLD chamber (IPLD).21 More general, tremendous performance differences by several orders of magnitude were reported in literature for LSC thin film electrodes of nominally identical composition.13,17,19,21−32 This may be partly caused by different growth conditions, leading to nonequilibrium defects, such as grain boundaries or dislocations and possibly also to different cation stoichiometries.", "However, also any condition a freshly prepared PLD film is exposed to before its first characterization may contribute to these substantial differences; this includes cooling after preparation, exposure to ambient air for some time after deposition, current collector deposition or micropatterning (if required), mounting in a sample holder, heating to the measurement temperature in an atmosphere with possible impurities, etc.", "All these steps may modify the surface and lead to an ill-defined state of LSC (or any other) thin film electrode.", "Accordingly, comparability of properties found in different laboratories as well as comparability between different materials is challenging due to ill-defined pretreatments of “as-prepared” films.", "Also studies on the film thickness dependence of electrochemical properties and on the role of strain may be affected if changes after preparation are not avoided.", "This clearly indicates the need for improved methods to get reliable and reproducible data on the “virgin properties” of freshly prepared thin films.", "In this contribution, we introduce such a method and directly monitor the electrochemical properties of mixed ionic electronic conducting LSC thin films during their growth in the PLD setup by using impedance spectroscopy (IPLD).", "This approach allows the highly reproducible analysis of the electrochemical surface polarization resistance of virgin LSC thin films during deposition.", "Hence, the preparation conditions during thin film growth are the only variables that may still affect the measured properties.", "The very low LSC surface polarization resistance obtained in these experiments also indicates a still unexploited potential of the fast oxygen exchange kinetics of LSC thin films.", "Equivalent circuit models are applied to determine the oxygen exchange resistance, the interfacial capacitance and the chemical capacitance of growing films, the latter revealing information on the defect chemistry.", "Thickness dependencies of these quantities were examined for 25 different deposition stages, starting from the earliest stages of film growth below 4 nm thickness to a fully grown thin film of 100 nm.", "Problems in determining accurate oxygen exchange properties for the thinnest layers are discussed.", "Moreover, the influence of lattice mismatch on the electrochemical film properties is studied by comparing films on yttria stabilized zirconia (YSZ) to epitaxially grown LSC on La0.95Sr0.05Ga0.95Mg0.05O3−δ (LSGM) single crystals.", "The measured kinetic data are discussed in the context of oxygen exchange properties of LSC reported in literature.", "Methods Sample Preparation For most experiments (100) oriented yttria stabilized zirconia (YSZ, 9.5 mol % Y2O3, Crystec GmbH, Germany) single crystalline substrates were used with a thickness of 0.5 mm and a size of 5 × 5 mm2.", "Some experiments were performed on (100) oriented La0.95Sr0.05Ga0.95Mg0.05O3−δ (LSGM) single crystals of the same size, synthesis and preparation are detailed in ref (33).", "Five nm Ti (4N5; FHR Anlagenbau GmbH, Germany) and 100 nm Pt (3N5; SPM AG, Liechtenstein) thin films were deposited onto the electrolyte single crystals by a sputter coater (LS320S, Von Ardenne, Germany).", "Sputtering was performed at room temperature in 8 μbar Ar atmosphere.", "A rectangular grid structure (100 μm hole/25 μm stripe width) was then prepared on almost the entire YSZ/LSGM surface by lift-off photolithography.", "This Ti+Pt grid serves as current collector for the counter electrode (CE), see Figure S1a.", "(The thin Ti layer is used to improve adhesion of Pt to YSZ, while the electrical current collector properties are determined by the Pt layer).", "The sample was flipped and the process was repeated to yield another current collecting Ti+Pt grid (11/9; 35/15 or 100/25 μm hole/stripe width) over 4.5 × 4.5 mm2 on the corresponding electrolyte surface (Figure S1b).", "On this grid, the LSC working electrode (WE) was deposited (see below) and its electrochemical properties were characterized by impedance spectroscopy during growth.", "Targets for preparation of LSC thin films by pulsed laser deposition (PLD) were synthesized from powders prepared by a modified Pechini synthesis.34 La2O3, SrCO3 and Co powders (all Sigma-Aldrich, 99.995%) were individually dissolved in nitric acid, mixed in appropriate ratios and citric acid (TraceSELECT, 99.9998%) was added for chelation.", "After evaporation of water a viscous foam forms, which spontaneously decomposes upon further heating.", "The obtained intermediate product was calcined at 1000 °C, followed by isostatical pressing (∼310 MPa) of the powder to a pellet and a sintering procedure at 1200 °C for 12 h in air, thus yielding a La0.6Sr0.4CoO3−δ target for PLD.", "The exact film composition (La0.607±0.008Sr0.396±0.004Co0.996±0.005O3−δ) was determined from thin films grown by standard PLD on YSZ.", "Those were dissolved in hydrochloric acid and analyzed by Inductively Coupled Plasma–Optical Emission Spectroscopy.", "First, a microporous LSC film22 was deposited on the CE current collector grid using PLD.", "Ablation of the target material was carried out by a KrF (λ = 248 nm) excimer laser (Lambda COMPexPro 201F) operated at a pulse repetition rate of 5 Hz, a pulse duration of 50 ns and a laser fluence of approximately 1.5 J·cm–2 at the target.", "The atmosphere was set to 400 μbar oxygen partial pressure O2 and the substrate was heated to a surface temperature of approximately 450 °C.", "These preparation conditions lead to films with columnar structure and significant inner surface, which lead to a particularly low polarization resistance of the resulting counter electrode.22,35 By applying 9000 laser pulses to the LSC target, a thin film of approximately 300 nm thickness was grown on the substrate (substrate to target distance = 5 cm).", "After deposition, the sample was cooled in the deposition atmosphere at a cooling rate of 12 °C·min–1 and the side faces of the YSZ crystal were gently ground to remove any residual LSC or Ti+Pt.", "It is noteworthy that the sample surface was never exposed to “cleaning” treatments after electrode deposition in order to avoid any contamination from solvents including H2O.19 In situ Impedance PLD Measurements The in situ impedance PLD (IPLD) setup is sketched in Figure 1a.", "A quartz plate is placed on top of the uncovered Pt heating wires for electronic isolation, followed by a Pt sheet, which is pinned down by a corundum plate with a 5 × 5 mm2 opening in the center.", "A sample with a CE and a current collecting grid for the WE (see above) is placed into the opening such that the CE is in direct contact with the underlying Pt sheet.", "The sample is covered by a second corundum plate with a smaller opening (∼4.2 × 4.2 mm2) serving as a mask during PLD deposition of the working electrode.", "This mask is exactly center-aligned by two small corundum pegs (both corundum plates have drilled holes).", "Finally, the upper Ti+Pt grid, that is, the current collector of the working electrode to be deposited, is contacted in the center by a Pt tip attached to a movable Cu arm, see photographs in Figure 1b and 1c.", "This electrical contact between Pt tip and Ti+Pt current collector grid remained intact during the entire experiment, that is, also during film deposition.", "The main difference compared to the IPLD setup presented in ref (21) is the use of the additional corundum masks for electronic isolation.", "Otherwise, deposition of a MIEC would lead to a short-circuit between WE and CE, since electrode material is not only deposited on the top but also on the outer sides of the sample.", "Figure 1 In situ impedance setup for PLD (IPLD): (a) Sketch of the entire setup; Ti+Pt grids (5 + 100 nm thickness) are prepared on both sides of the 5 × 5 mm2 electrolyte single crystal (500 μm thickness) and a porous LSC counter electrode (CE) is deposited by PLD on the back side.", "The sample is then put on a Pt sheet on top of the PLD heater and a corundum sample holder is placed around it.", "Finally, a corundum mask is placed on top of the sample holder and the Pt grid is contacted by a Pt tip in the center of the sample.", "(b) Setup from above.", "(c) Pt tip contacting the Pt current collector grid; the opening of the masks is also clearly visible.", "Prior to the actual IPLD experiments, the LSC target was ground, inserted into the PLD, and ablated for 60 s at 5 Hz in 40 μbar O2 at room temperature.", "Then, the PLD recipient was opened and the sample, masks and Pt tip were positioned as described above at a sample to target distance of 6 cm.", "Subsequently, the recipient was evacuated and the atmosphere was set to 40 μbar O2 before heating the sample to 600 °C.", "The temperature was controlled by measuring the high frequency intercept in Nyquist plots of impedance measurements.", "At ∼600 °C this resistance is mainly caused by the ion conduction in the YSZ or LSGM single crystal, with minor contributions from the electronic sheet resistance of the Ti+Pt grid and the serial 2-point Pt wire resistance.", "The serial 2-point Pt wire resistance (about 2 Ω at 600 °C) was separately measured by placing the Pt tip directly on the CE Pt-sheet and the electronic sheet resistance of the Ti+Pt grid was estimated for each grid geometry according to eq S2.", "Hence, the temperature dependent ionic oxygen transport resistance could be determined from the measured high frequency intercept.", "The known conductivity–temperature relationship of our YSZ36 and LSGM33 single crystal electrolytes was then used to determine and control the temperature throughout the experiments (see section S-3 for more details).", "The laser repetition rate was set to 1 Hz for deposition sequences of 25, 50, 100 laser pulses and increased to 2 Hz for ablations with 200, 250, or 500 laser pulses.", "The surface area of the WE shadowed by the contact tip during material deposition is below 4% of the total area (Figure S1c and d).", "This was estimated from microscope images (color contrast) after growing a complete LSC electrode (∼100 nm) on top of the YSZ single crystal.", "In the further analysis any substantial effect of this shadowed film region was neglected.", "The impedance measurements were performed by a Novocontrol Alpha A High Performance Frequency Analyzer in the frequency range from 106 to a minimum of 10–2 Hz with a resolution of five points per decade and an alternating voltage of 10 mV (rms) applied between the WE and the CE.", "After each deposition sequence, up to three spectra (each taking more than 10 min of measuring time) were measured subsequently and those were generally in excellent agreement.", "This guarantees that any resistance and capacitance changes found after additional deposition steps are true effects, not altered by any degradation processes, and that sufficiently mobile defects, such as oxygen vacancies in the LSC thin film are equilibrated.", "LSC Growth Rate A profilometer (DekTakXT, Bruker, USA) was used to determine the LSC film thickness grown on YSZ and LSGM substrates to calculate the growth rate (pulses/nm).", "For this procedure about 5000 laser pulses at 2 Hz repetition rate were applied to the respective targets and the films were grown under the same PLD conditions as for the IPLD experiments (600 °C substrate temperature, 40 μbar O2 atmosphere).", "Subsequently, photolithography and chemical etching were employed to remove parts of the thin films, thus generating multiple steps which could be analyzed.", "A nominal LSC film thickness of about 100 ± 7 nm was found for both substrates, which yields a growth rate of about 0.02 nm/laser pulse, assuming thickness independent film growth.", "Consequently, the amount of applied laser pulses (assuming linear film growth) was translated to a nominal film thickness for the growing LSC thin films.", "The PLD growth conditions are the same as in earlier studies on similar LSC films13,19,28,33 and the corresponding films have proven to be highly crystalline and textured with preference of the (100) and (110) direction on YSZ13,19 and epitaxial (100) growth on LSGM.33 Ex Situ Resistivity and Morphology Measurements In-plane resistivity measurements of LSC thin films were performed in a separate setup.", "Four platinum needles were placed on LSC thin films deposited onto a 10 × 10 mm2 YSZ single crystal close to the sample edge to meet the prerequisites of the van der Pauw method.37 A series of LSC thin films with different nominal thicknesses (1–100 nm) was investigated.", "The setup was uniformly heated in a tube furnace and the temperature was measured by means of an encapsulated type K thermocouple positioned adjacent to the sample.", "A mixture of high purity N2/O2 was used to realize an oxygen partial pressure of 0.21 bar.", "A precision voltage source (2410, Keithley Instruments, USA) and a multimeter (2000, Keithley Instruments, USA) were employed for these conductivity measurements.", "Atomic force microscopy (AFM) was performed after depositing LSC thin films onto a LSGM or YSZ substrate to analyze the different surface microstructures (Figure S3).", "A Nanoscope V multimode setup was utilized in tapping mode, equipped with silicon tips.", "In general, a scan rate of 2 Hz and a resolution of 512 × 512 pixels over a scan area of 1 × 1 μm2 were chosen.", "The collected data were evaluated and plotted by Bruker’s NanoScope Analysis 1.3 software.", "Results and Discussion Qualitative Impedance Changes during the First Stages of LSC Film Growth The initial sample consists of a Ti+Pt grid on top of the YSZ single crystal with a porous LSC counter electrode (CE).", "After mounting it in the IPLD setup (more details in Methods) and thermal equilibration at 600 °C in 40 μbar O2 an impedance spectrum was measured, see Figures 2a and S2.", "The impedance is characterized by a high frequency intercept on the x-axis (>50 kHz) followed by two depressed semicircles at medium (50 kHz–1 Hz) and low (1 Hz–10 mHz) frequencies.", "The high frequency intercept on the real axis of the Nyquist plot (Rhf ∼ 55 Ω) can be largely attributed to the oxide ion conduction in the electrolyte (Rion,YSZ > 0.8 × Rhf) with small contributions from the electronic sheet resistance of the Ti+Pt grid (Reon,grid = ∼5–10 Ω) and the wiring resistance (Reon,wire = ∼2 Ω), see section S-4 for more details.", "This spectrum was fitted to an Rhf – Rmf∥CPEmf – Rlf∥CPElf equivalent circuit (CPE = constant phase element), see Figure S2.", "Averaged fit results of six samples were normalized to the triple phase boundary (TPB) length, as well as to the surface area (SA) of the metal grid and the resulting mean values are given in Table 1.", "Figure 2 Impedance of a growing LSC thin film, 0–150 laser pulses (p).", "Representative Nyquist plots of samples with a (35/15 μm) Ti+Pt current collector grid for the top electrode.", "An increasing amount of LSC is then grown by applying 0–125 laser pulses onto the LSC target (25 pulses correspond to nominally 0.5 nm LSC) and impedance spectra are measured in situ at 600 °C and 40 μbar O2 (a).", "After applying 150 laser pulses (nominally 3 nm LSC), the impedance spectra are primarily determined by the grown LSC thin film (see text) and the simplified equivalent circuit shown in the figure can be used to extract physically meaningful parameters (b).", "Table 1 Resistive and Capacitive Values for Six 5 + 100 nm Ti+Pt Thin Film Grids of Different Geometries, Normalized to the Triple-Phase Boundary Length (TPB) or Surface Area (SA) Rmf·SA [Ω cm2] Rmf·TPB [Ω cm] Cmf/SA [F/cm2] Rlf·SA [Ω cm2] Rlf·TPB [Ω cm] Clf/SA [F/cm2] 7.5 ± 1.8 × 102 8.3 ± 2.3 × 105 1.4 ± 1.1 × 10–4 1.1 ± 1.0 × 104 1.2 ± 1.1 × 107 5.2 ± 0.8 × 10–4 Owing to the low polarization resistance of the CE22,35 both arcs can be attributed to the Ti+Pt grid electrode.", "The TPB related low frequency resistance of the Ti+Pt grid is close to the oxygen exchange resistance expected for micropatterned Pt thin film electrodes at 600 °C in air (1.0 × 107 Ωcm).36 Measured capacitances are in the range of several tens or even hundreds of μF/cm2 in parallel to the oxygen exchange path.", "Comparable values have also been reported for different metal electrodes sputtered on YSZ and are usually attributed to a capacitance at the electrolyte/electrode interface.38−41 Hence, the initial current collector grid seems to be similar to TPB active Pt electrodes on YSZ, with the resistance being due to oxygen exchange close to the TPB and the capacitance originating from the entire interfacial area.", "A more detailed analysis is beyond the scope of this paper, since the metal grid only acts as current collector in our experiments, at least after 3 nm of LSC were deposited, see explanation below.", "Strong changes of the impedance spectra are observed when depositing small amount of LSC, see Figure 2a.", "The total resistance of the sample decreases by almost 2 orders of magnitude from 37.5 kΩ down to 0.4 kΩ after applying 150 laser pulses to the LSC target (i.e., for 3 nm nominal LSC film thickness), cf.", "Figure 2b.", "Moreover, the shape of the impedance spectra changes as well.", "The two semicircles found in the beginning become more and more depressed and uncommonly (tail-like) shaped, but after applying 150 laser pulses on the LSC target a “regularly-shaped” impedance spectrum is again found, now with three semicircles.", "These observations indicate that already when depositing very small amounts of LSC a much faster oxygen exchange path becomes active.", "Since LSC is an electrode material with oxygen exchange proceeding via the bulk path, it is reasonable to assume that establishing this pathway upon growing the electrode is responsible for the drastic decrease of the polarization resistance.", "For very small pulse numbers there might still be a contribution from the current collector grid because of incomplete covering by LSC.", "However, after depositing about 3 nm LSC (150 pulses), the resistance has decreased to less than 1% of its original value and the transition from a TPB active metal grid electrode to a purely MIEC bulk path active LSC electrode is certainly completed.", "Covered by LSC, the metal grid is no longer contributing to the oxygen exchange reaction but only serves as current collector that supplies electrons to the reaction sites at the LSC surface.", "The following scientific questions can therefore be addressed by further film growth and IPLD analysis: i.", "What is the absolute value of the oxygen surface exchange resistance of LSC (RLSC, surf exch) immediately after preparation?", "ii.", "How reproducible is this value?", "iii.", "Does the oxygen surface exchange resistance of LSC change with increasing layer thickness?", "iv.", "Does the volume specific chemical capacitance and thus the concentration of defects depend on LSC film thickness?", "v.", "Is there an additional interfacial contribution to the capacitance of LSC thin films?", "vi.", "How does the surface exchange resistance and the chemical capacitance of freshly prepared LSC depend on the substrate, for example, on strain?", "To answer these questions, we need to extract the corresponding resistive and capacitive parameters of LSC thin film electrodes from the impedance spectra.", "Analysis of Impedance Spectra For analyzing the spectrum measured after 150 pulses (3 nm LSC), and spectra of thicker films, we have to consider all kinetic processes involved in this experiment.", "First of all, we have to keep in mind that oxygen exchange on dense LSC thin film electrodes takes place via the so-called bulk path with oxygen reduction/evolution at the surface, ion transport through the film and interfacial ion transfer from electrode into the electrolyte.8,14 Moreover, we have to take into account that the oxygen exchange path through the LSC bulk not only requires an ionic connection to the electrolyte but also an electronic connection to the current collector grid.", "During the in situ growth experiment, LSC is deposited on both the Ti+Pt grid and on the electrolyte in between the metal stripes.", "Since, the metal grid is considered to be blocking for oxygen diffusion (see above), LSC deposited on top of the grid is virtually ionically disconnected from the electrolyte, only a very resistive ionic in-plane path to YSZ exists, provided the “side walls” of the current collector grid are also covered by LSC.", "Thus, practically only LSC deposited in the mesh holes of the grid and thus in direct contact with YSZ can participate in the oxygen exchange reaction.", "The sketch in Figure 3 indicates the geometry of a mesh-hole cross-section after depositing some LSC and illustrates the oxygen exchange path, together with a proposed equivalent circuit.", "The latter is derived from the general description of mixed ionic and electronic conductors (MIEC) by Jamnik and Maier42 (cf., also ref (43)).", "It includes the in-plane electronic resistances of Pt (Reon,Pt) and LSC (Reon,LSC), the ionic resistance of YSZ (Rion,YSZ), and the oxygen surface exchange resistance of LSC (Rsurfexch,LSC).", "In accordance with other studies on LSC thin films the ionic across-plane transport resistance is neglected;19,29,30 also the ionic interfacial transfer resistance between LSC and YSZ is neglected because of absence of a corresponding impedance arc in thicker films, see below.", "Figure 3 Mesh-hole cross-section after depositing some LSC on as-prepared samples.", "The oxygen exchange path is illustrated together with a 3D equivalent circuit model that allows to fully describe resistive and capacitive contribution expected after depositing >3 nm of LSC.", "Capacitive behavior can originate from the interfacial capacitance between the Ti+Pt grid and YSZ (Cdl,Pt), the interfacial capacitance between LSC and YSZ (Cdl,LSC), and the chemical capacitance of the LSC bulk (Cchem,LSC).", "The latter two capacitances, however, are in parallel in the model of a MIEC electrode42 and thus cannot be separated.", "In principle, an exact impedance model for analyzing the impedance data may thus be established.", "However, because of the complexity of this circuit, particularly because of the transmission lines involved, a quantitative analysis would be very challenging.", "Instead a simplified equivalent circuit (Figure 2b) was used to analyze the impedance spectra obtained after depositing 3 nm or more LSC.", "This is considered as a very reasonable approximation, provided the arcs are fairly well separated.", "At high frequencies, all capacitors mentioned above exhibit low impedances and only a serial high frequency offset resistance (Rhf) is measured.", "This was already discussed above; it is dominated by the ionic resistance of YSZ but also includes the electron sheet resistance in the Pt grid and a Pt-tip contact resistance.", "The current can flow via path 1 sketched in Figure 3.", "For Cdl,Pt being smaller than the parallel connection of the two LSC related capacitances, lower frequencies result in a current path via the two still open LSC capacitors (path 2 in Figure 3).", "However, then the electronic sheet resistance in the LSC comes into play and an arc results in the impedance spectrum (50 kHz–0.5 kHz).", "To a first approximation this switch of the current path can be described by a parallel connection of a capacitor due to Cdl,Pt and a resistor reflecting contributions of Reon,LSC.", "In the simplified circuit the corresponding arc is represented by the effective working electrode resistor RWE, sheet and a constant phase element CPEcc, from which capacitances can be deduced, see below.", "For even lower frequencies (0.5 kHz–1 Hz) also the LSC related capacitors achieve high impedance values, the current now takes path 3 across the oxygen exchange resistance and another arc results which can be approximated by the effective oxygen exchange resistance RWE,surfexch and CPEWE.", "In particular, RWE,surfexch and CWE (from CPEWE) give insight into the kinetic and thermodynamic properties of our growing LSC thin film, respectively.", "A very similar situation was already considered in ref.43 for a MIEC under reducing conditions.", "The last semicircle like feature (<1 Hz) is determined by the oxygen exchange kinetics at the counter electrode (RCE), in parallel to the rather large chemical capacitance of the comparatively thick CE, represented by CPECE.", "All constant phase elements can be used to calculate capacitances according to ref (44) by ZCPE = Q–1(iω)−n and C = (R1–n·Q)1/n from fitting parameters Q and n.", "On the basis of this interpretation of impedance spectra, we can now quantitatively analyze the absolute values and film thickness dependences of all sample properties for LSC films beyond 3 nm thickness, i.e.", "LSC prepared by more than 150 pulses (next two subsections).", "This analysis also further illustrates the appropriateness of the suggested impedance interpretation.", "Fit Parameter Changes during Further Film Growth Figure 4 displays spectra found for LSC layers prepared by up to 5000 laser pulses, corresponding to a film thickness of about 100 nm.", "With continuous film growth, the diameter of the high frequency semicircle decreases until it can no longer be fitted properly for thin films with thicknesses of 20 nm or more; RWE,sheet in the equivalent circuit is then fixed to zero.", "For very thin films, the medium frequency semicircle also decreases with increasing film thickness, but then reaches a constant level for thicker films.", "The low frequency semicircle remains almost unaffected by the deposition of LSC, in accordance with its interpretation as the counter electrode impedance.", "Parameterization of the impedance spectra was done by complex nonlinear least-squares fitting using the equivalent circuit in Figure 2b and results are summarized in Figure 5a.", "Figure 4 Impedance spectra for a growing LSC thin film, 150–5000 laser pulses, that is, 3–100 nm.", "Representative Nyquist plots showing the continuous growth of an LSC thin film from 3–4.5 (a), 5–20 (b), and 40–100 nm (c) on a (35/15 μm) Ti+Pt grid.", "The LSC thin film is grown (0.02 nm/laser pulse) and electrochemically measured in situ at 600 °C and 40 μbar O2 by IPLD.", "All experimental data are fitted to the equivalent circuit shown in Figure 2b.", "Figure 5 Resistances (a) and capacitances (b) of an LSC thin film grown and measured in situ by IPLD.", "The LSC thin film was deposited at 600 °C in 40 μbar O2 on YSZ single crystal electrolyte with a (35/15 μm) current collector grid.", "The corresponding impedance spectra are shown in Figure 3 and 5 and values were extracted by the equivalent circuit shown in Figure 3b.", "As already mentioned, RWE,surfexch, strongly decreases during the first few hundred laser pulses and reaches a constant value after about 20 nm.", "At first sight, this seems to indicate a severe film thickness dependence of the LSC oxygen exchange kinetics.", "However, simultaneously RWE,sheet strongly decreases with increasing thickness and reaches zero for almost the same amount of laser pulses and thus layer thickness.", "The similar behavior of these two resistances indicates that the parameters are correlated.", "We first consider RWE,sheet in more detail.", "According to our interpretation, RWE,sheet is primarily determined by Reon,LSC, the electronic sheet resistance of LSC between the metal stripes, see Figure 5.", "For simple geometric reasons this value should indeed exhibit a decrease for increasing thickness.", "However, when assuming a typical electronic conductivity of LSC (1000 S/cm13) numerical finite element simulations (COMSOL) for the given geometrical parameters could not reproduce the absolute value of RWE,sheet at the beginning of the experiment.", "Hence, a further effect has to come into play.", "Additional ex situ measurements on very thin LSC films were conducted using Van der Pauw’s method to measure the true in-plane conductivity (electronic conductivity), see Figure 6.", "A strong decrease of the nominal electronic conductivity by orders of magnitude is observed when the film thickness is reduced below a critical film thickness of about 20 nm (1000 laser pulses).", "This is in excellent accordance with the very pronounced increase of RWE,sheet below 20 nm resulting from our analysis of in situ impedance experiments.", "Most probably, very thin layers have a complex and possibly islands-like morphology rather than an exactly homogeneous thickness.", "Thus, tortuosity plays a significant role and enhances the LSC sheet resistance especially in the early stages of thin film growth.", "Figure 6 Total (effective) conductivity (σeon ≫ σion) of LSC thin films depending on the number of applied laser pulses, that is, film thickness.", "The conductivity was measured in van-der-Pauw geometry at 600 °C and 10 μbar p(O2).", "Between 50 and 5000 laser pulses were applied to a LSC target in order to grow films of 1 to 100 nm nominal thickness.", "This reduced in-plane electron conduction of very thin films directly affects RWE,surfexch.", "It limits the polarized electrode area and thus only LSC close to the metal grid participates in the oxygen exchange, while LSC surface further away from the current collector remains electrochemically inactive.", "Therefore, a higher nominal RWE,surfexch can be expected as long as a significant LSC sheet resistance exists.", "This is exactly what we see in Figure 5a: In the beginning, RWE,surfexch strongly decreases with increasing thickness.", "The LSC surface exchange resistance reaches a constant level when RWE,sheet has vanished, that is, when the entire LSC area between the metal stripes is polarized and thus active for the oxygen exchange.", "Hence, the sharp decrease of the measured polarization resistance does not indicate much higher catalytic activity for thicker films but primarily more active surface area.", "We have to conclude that the area specific oxygen exchange properties of very thin LSC films (<20 nm) cannot be extracted by this analysis, due to an unknown active area.", "Hence, also a true change of the surface exchange properties in very thin layers (e.g., due to different surfaces) cannot be excluded.", "For layers thicker than 20 nm, on the other hand, the surface exchange properties are thickness independent.", "Between 20 and 100 nm film thickness the capacitance CWE of the working electrode increases linearly with the number of applied laser pulses.", "However, a significant deviation from linearity to lower capacitance values occurs for thinner films (<20 nm), which cannot be clearly seen in Figure 5b due to log–log plotting of data but is explicitly addressed in the next sections.", "This behavior suggests that CWE is also influenced by a limited in-plane electron conduction.", "It is in accordance with measurements performed by Wedig et al. reporting a strong influence of the electrical sheet resistance on the chemical capacitance of Bi1–xSrxFeO3−δ thin films.45,46 Surprisingly, CCC also seems to show an increase with increasing film thickness.", "However, with decreasing size of the high frequency semicircle (cf., Figure 4) a significant error results from the fitting procedure (see large error bars in Figure 5b), which complicates proper evaluation and hinders a clear conclusion on its thickness (in-)dependence.", "Meanwhile, the counter electrode resistive (RCE,surfexch) and capacitive (CCE) quantities (Figure 5b) remain unaffected by the growth of the working electrode.", "Normalization to the grid-free area (0.17 cm2) of the counter electrode, i.e. the surface that participates in the oxygen exchange, reveals a remarkably low resistance of the microporous LSC of about 5.6 Ωcm2 at 600 °C and 40 μbar O2.", "Reproducibility and Quantitative Evaluation of the LSC Film Properties The electrochemical LSC thin film properties, RWE,surfexch and CWE were determined for two further thin films with different metal grid geometries.", "The results are shown in Figure 7a and 7b.", "The shape of the resistance-thickness curves for the (35/15 μm) current collector pattern is reproduced also for the other two geometries.", "In the beginning, a comparatively high RWE,surfexch is found for all grid geometries, which rapidly decreases while growing the first 10–25 nm of LSC on top.", "The decrease is followed by an almost ideal plateau in case of the (35/15 μm) and (100/25 μm) sample.", "For the LSC thin film with a very narrow grid (11/9 μm) the resistance still slightly decreases.", "The capacitance increases linearly for larger LSC thicknesses but exhibits a deviation from linearity with an x-axis offset for very thin films.", "Figure 7 Resistive (RWE,surf,exch) and capacitive (CWE = Cchem,LSC + Cdl,LSC) properties of growing thin films measured in situ by IPLD.", "Surface exchange resistance and capacitance of the LSC working electrode before (a, b) and after (c, d) normalization to the grid-free area, measured at 600 °C and 40 μbar O2.", "Three different rectangular metal grid geometries were employed (11/9, 35/15, or 100/25 μm hole/stripe width) to verify that only LSC in direct contact with the electrolyte participates in the oxygen exchange reaction.", "Figure 7c and 7d show the same results after normalization to the mesh hole area, that is, the area of LSC deposited directly on YSZ.", "For resistances as well as capacitances this leads to almost perfectly coinciding curves.", "This supports the assumption that indeed only LSC deposited directly on top of the electrolyte participates in the oxygen exchange and contributes to the capacitance.", "It also indicates the excellent reproducibility of the LSC film properties immediately after deposition.", "The slight drift to a lower specific resistance found with the narrow grid (11/9 μm) sample for increasing LSC thickness is most probably caused by the decreasing ionic sheet resistance above the metal current collector grid.", "Small parts of LSC above the metal grid and close to the LSC/YSZ interface might participate in the oxygen exchange as well and this becomes especially relevant for the finest grid.", "An increase of the active LSC area of a 100 nm thin film by activating a ∼500 nm wide LSC region above the current collector, that is, an effective mesh size of (12/8 μm) instead of (11/9 μm) would already lead to the same RWE,surfexch and CWE for all mesh geometries.", "An estimate of the decay length of the electrochemical activity can be found in the S-6.", "This effect becomes less important for larger mesh widths.", "However, a purely empirical correction of the values for different current collectors would add some arbitrariness and the area-specific values were thus not corrected in the further analysis.", "On the basis of these measurements, we can now answer questions i, ii, and iii raised above (reproducibility and absolute value of RLSC,surfexch ,as well as its thickness dependence).", "First, the agreement of the oxygen exchange resistances measured for different films is remarkable.", "When fitting the data to exponential decay functions (see lines in Figure 7c), an average oxygen exchange resistance of 2.04 ± 0.1 Ω cm2 is determined for a fully grown thin film (>50 nm) measured at 600 °C in 40 μbar.", "It should be noted that most studies on LSC polarization resistances, report variations in the range of a factor of 2 or more, even for nominally identical samples.8,26,30 The very high reproducibility found in our study can be most probably attributed to the type of experiment, with films never being exposed to other atmospheres or temperatures and being measured immediately after deposition.", "Second, the polarization resistance of 2.0 Ω cm2 value is impressively low, taking into account the very low oxygen partial pressure of 40 μbar used here.", "A more detailed discussion of this absolute value, also comparing this low polarization resistance with other literature values, can be found below.", "And third, these experiments again confirm that there is no thickness dependency of RWE,surfexch for films larger than 20 nm thickness.", "For a further analysis of the thickness dependent capacitances, CWE, we first normalize the raw data (Figure 7b) to the nominally active area, that is, to the area of LSC directly on YSZ (Figure 7d).", "Above ∼20 nm film thickness a linear relation is found for all three experiments and a linear fit leads to very similar slopes, on average to 1281 ± 39 F/cm3.", "This linearly growing contribution to CWE can be attributed to the chemical capacitance of the LSC film Cchem,LSC, which is a volume property of the electrode material and given by ref (33) 1with e being the elementary charge, A and t the electrode surface and thickness, and cO and μO the concentration and chemical potential of oxygen, respectively.", "This identification of the main contribution of CWE as the chemical bulk capacitance also justifies our interpretation of its parallel resistor RWE,surfexch as the oxygen surface exchange resistance: In accordance with the established models of mixed conducting electrodes,8,14,23,29,47 only the surface related resistance is in parallel to the chemical capacitance, provided ionic bulk transport is sufficiently fast, see Figure 3.", "However, this surface-related resistance can include contributions from several elementary steps without leading to additional arcs in impedance spectra.", "Accordingly, further statements on the exact mechanistic character of RWE,surfexch require more detailed studies, for example, on the p(O2) and overpotential dependence.48 Extrapolation of the linear fits (Figure 7d) leads to an intersection with the ordinate at very similar values (1012 ± 253 μF/cm2), see also the plot of the normalized WE capacitance for the first nanometers of thin film growth in Figure 8a.", "The interpolated ordinate intersect of about 1000 μF/cm2 is interpreted as the thickness-independent interfacial capacitance, CdlLSC, which is in parallel to the measured chemical capacitance of LSC.", "Since the chemical capacitance and the interfacial capacitance are both in parallel to our surface exchange resistance (see ref (42) and Figure 3) a discrimination is only possible based on the thickness dependency of Cchem,LSC.", "This analysis thus answers questions iv and v mentioned above (thickness dependence of Cchem and additional capacitive contribution of the interface).", "Figure 8 Capacitance of the working electrode CWE (a) and of the oxygen exchange resistance as well as of CWE (b) in the beginning of thin film growth.", "Part a is a zoom of measured data and linear fit of Figure 7d.", "The intersection between ordinate and the three fit lines allows determining the interfacial capacitance between LSC and YSZ.", "The ratios in part b reveal the similarity between deviations of resistive and capacitive properties from the values expected by extrapolation of results found for thicker layers (RWE,surfexch,expec = 2.02 Ω cm2 and CWE,expec = 1012 μF/cm2 + 1281 F/cm3 × thickness).", "If an additional interfacial resistance were present, the interfacial capacitance could be obtained from the resulting separate impedance arc.", "This was the case for the interfacial capacitance reported by Baumann et al.14 (40 μF/cm2) measured for La0.6Sr0.4Co0.8Fe0.2O3−δ electrodes on YSZ electrolyte at 750 °C in air and also for a not yet interpreted capacitance (19000 μF/cm2) found in ref (13) for La0.6Sr0.4CoO3−δ on YSZ at 600 °C in 250 μbar p(O2).", "The latter showed a behavior typical for chemical capacitances, for example, p(O2) dependence.", "The origin of this capacitance is still unknown, but future IPLD experiments in varying p(O2) atmospheres or under DC polarization might give insights into the nature of Cdl,LSC.", "For thinner films (<20 nm) not only RWE,surfexch but also CWE deviates from model expectations, that is, from a linear fit.", "For CWE, we find an apparent x-axis offset (instead of a y-axis offset), followed by an asymptotic increase of CWE.", "We already concluded that for thinner films an increasing electronic sheet resistance leads to an incomplete electrode polarization.", "This should cause not only an increased RWE, surfexch, but also a decreased CWE compared to fully polarized layers.", "Such a simultaneously appearing nonideality is indeed present and becomes obvious when comparing measured and expected values of the oxygen exchange activity (1/RWE,surfexch) and CWE, see Figure 8b.", "There, the ratio is shown between measured RWE,surfexch and thickness-independent RWE,surfexch,expec = 2.02 Ωcm2, as well as between CWE and CWE,expec = 1012 μF/cm2 + 1281 F/cm3 × thickness [cm].", "For all thin films, a very steep increase of the respective ratios is observed in the beginning, which levels out after 20–30 nm film thickness.", "This very similar behavior of a bulk property (Cchem,LSC) and a surface property (RLSC,surfexch) suggests that even below 20 nm film thickness (down to 3.5 nm) most properties of LSC do not depend much on the film thickness.", "Rather the virtual thickness dependence of both parameters observed here is largely caused by an incomplete current collection for very thin films.", "Strained LSC Thin Films on LSGM The high reproducibility of the properties found in our IPLD measurements allows a very accurate analysis of the role of the substrate on LSC film properties (see question vi mentioned above).", "While growth on YSZ leads to nanocrystalline LSC layers with several orientations, (La, Sr)(Ga,Mg)O3−δ (LSGM) single crystalline electrolytes allow growth of strained epitaxial LSC layers.", "A detailed structural and electrochemical study on La0.95Sr0.05Ga0.95Mg0.05O3−δ single crystals was presented elsewhere, including growth of strained LSC film (∼0.8% tensile strain at room temperature) using similar PLD conditions.33 Qualitatively, the impedance spectra (Figure S4) obtained during LSC film growth were similar to the ones presented in Figures 2b and 4.", "A smaller high frequency intercept on the x-axis is found, due to a higher ionic conductivity of LSGM, followed by 2–3 arcs representing RWE,sheet (again only visible in the beginning of film growth), RWE,surfexch and RCE,surfexch.", "Hence, all data could again be fitted to the equivalent circuit shown in Figure 2b and the extracted quantities for two LSC/LSGM samples are compared to the LSC/YSZ samples in Figure 9.", "Figure 9 Resistive (RWE,surf,exch) and capacitive (CWE = Cchem,LSC + Cdl,LSC) properties of thin films growing on different substrates (LSGM vs YSZ) measured in situ by IPLD.", "Surface exchange resistance (a) and capacitance (b) of the LSC working electrode normalized to the grid-free area and measured at 600 °C in 40 μbar O2.", "In accordance with the observations for LSC on YSZ, a steep decrease of RWE,surfexch in the beginning of film growth is also measured for LSC on LSGM, followed by a saturation for films of about 20 nm thickness.", "Hence, the electronic sheet resistance in the beginning of film growth is again considered to be the reason for the decrease.", "A lower oxygen exchange resistance of 1.04 ± 0.02 Ωcm2 is reproducibly found for LSC on LSGM measured at 600 °C and 40 μbar O2.", "This indicates enhancement of the oxygen exchange kinetics by a factor of ∼2 for LSC films on LSGM compared to films on YSZ.", "This may be a direct consequence of the tensile strain in LSC.", "Faster chemical oxygen exchange coefficients for tensile strained LSC thin films deposited on STO were already measured by XRD49 and isotope exchange experiments.50 Moreover, a 1.6 higher chemical capacitance is determined for LSC on LSGM (2033 ± 21 F/cm3, Figure 9b) compared to YSZ (1281 ± 39 F/cm3).", "Hence, the tensile strain seems to cause a significant increase of the “effective concentration” of oxygen vacancies that determine the chemical capacitance of LSC.", "The latter is in agreement with theoretical and experimental work suggesting that tensile in-plane lattice strain decreases the vacancy formation energy and thus increases the vacancy concentration.51−53 However, also more indirect effects of the different substrates on film growth might play a role, particularly for RWE,surfexch, such as a different surface structure and chemistry of LSC on YSZ and LSGM.", "Usually, strain relaxation is expected to take place above a certain critical thickness.", "The expected in-plane compressive strain is comparably small (0.3% at 600 °C), calculated from lattice constants33 and thermal expansion coefficients.54,55 To the best of our knowledge, critical thicknesses of LSC on LSGM are not reported yet.", "However, SrTiO3 films, another perovskite-type oxide, deposited by molecular beam epitaxy on La0.7Sr0.3Al0.65Ta0.35O3 or DyScO3 lead to slightly larger strain values (−0.95% and 1.09%) and studies suggest a critical thickness of 30–180 nm.56,57 For larger strains, for example, LaAlO3 deposited on SrTiO3 (3.17%) by PLD, strain relaxation occurs earlier (20–50 nm).58 In our study, neither the surface exchange resistance (Figure 9a), saturating to a constant level, nor the electrode capacitance (Figure 9b), increasing linearly with increasing film thickness, give any evidence of thickness dependent strain relaxation.", "Hence, the critical thickness possibly exceeds the film thicknesses used here and our entire LSC films remain slightly strained.", "Also in our previous XRD study of 50 nm thin LSC films on top of LSGM, or on highly strained 20 nm thin LSC films deposited on SrTiO3 or LaAlO3,50 no relaxation was observed.", "However, the electrochemical properties found here are in contradiction to measurements reported in ref.23 for epitaxially grown, tensile strained La0.8Sr0.2CoO3-δ thin films deposited on GDC/YSZ.", "There, the oxygen exchange resistance of thinner films (20, 45, 135 nm) decreased and also significant differences of the volume specific chemical capacitance between the samples were reported (not following any thickness trend).", "We assume that discrepancies may come from the fact that our films were never exposed to any thermal cycling (cooling from PLD preparation temperature, heating for impedance measurement).", "In addition, other electrode preparation steps might induce changes of RWE,surfexch or Cchem and can thus alter comparability of different studies.", "Measurements in the IPLD setup seem to be particularly suited also for electrochemical investigations of substrate effects, including effects of lattice strain.", "Oxygen Surface Exchange Kinetics of LSC—A Literature Comparison Finally, we want to assess the measured polarization resistance of a freshly prepared LSC surface in the context of existing literature data.", "Numerous studies already investigated the oxygen exchange kinetics of LSC, but a large discrepancy between the reported values can be found.", "For the sake of simplicity, we only consider supposedly dense thin films prepared by pulsed laser deposition, which reliably allows relating the measured polarization resistance to the active surface area.", "Further, only studies reporting oxygen exchange coefficients (kq) or oxygen surface exchange resistances (Rsurfexch) derived by electrochemical methods are considered.", "We also focus primarily on the values reported prior to any degradation during the measurements.", "However, owing to the often unknown prehistory, this does not mean that no degradation has taken place before the measurements.", "For comparison, also exemplary resistances of degraded samples are considered.", "Three different LSC compositions (La0.8Sr0.2CoO3−δ, La0.6Sr0.4CoO3−δ, and La0.5Sr0.5CoO3−δ) are frequently investigated.", "Often, a higher Sr concentration is believed to accelerate the oxygen exchange kinetics at the expense of thermodynamic stability of LSC.59 However, recent studies by Crumlin26 and la O’23 compared similarly prepared La0.8Sr0.2CoO3−δ and La0.6Sr0.4CoO3−δ thin films and did not confirm a significant kinetic difference.", "This might again be due to the multiple effects affecting the polarization resistance mentioned in the introduction.", "Any comparison of data is further complicated, because various temperatures and oxygen partial pressures were used in all studies.", "Hence, normalization to a reference set of thermodynamic parameters is highly beneficial and a temperature of 600 °C and an oxygen partial pressure of 0.21 bar are chosen, since these were often experimentally applied and are in a relevant range for application of LSC, for example, in solid oxide fuel cells.", "Normalization of the oxygen surface exchange kinetics was performed as follows.", "Temperature: An Arrhenius-type dependence of the oxygen surface exchange kinetics was experimentally confirmed in many studies between 450 and 750 °C and activation energies of 1.26,13 1.3,8,24 and 1.3531 eV were determined for LSC thin films.", "A mean activation energy of 1.3 eV was chosen for extrapolation of the experimental data to the reference state.", "Oxygen partial pressure: A linear relationship in log Rsurfexch versus log p(O2) plots is often found with a negative slope m of 0.41,27 0.57,24 0.63,23 0.65,13 0.66,30 0.72,26 or 0.8.32 The meaning of this slope can be very complex and it should be emphasized that unambiguous interpretation in terms of a rate limiting reaction step is very challenging.48,60,61 A mean negative slope of 0.63 is used to account for different oxygen partial pressures in experiments.", "An overview of measured and extrapolated oxygen surface exchange resistance is given in Table 2.", "At a first glance, the tremendous difference of at least 3 orders of magnitude between Rsurfexch values (5 × 10–1–712 Ωcm2, excluding studies marked with an asterisk) obtained in different studies becomes apparent.", "Even if one attempts to normalize the results for each study to an individual combination of minimum and/or maximum values of the activation energy and partial pressure dependence m (mentioned above) in a way that calculated absolute Rsurfexch values move closer together, the discrepancy of 2.5–3 orders of magnitude is still found.", "Therefore, normalization cannot be held responsible for the large scatter.", "Table 2 Oxygen Surface Exchange Resistances of Dense La1–xSrxCoO3−δ Thin Films Deposited by PLD Measured at Different Conditions by Several Authorsa study electrode setup + annealed?", "La1–xSrxCoO3−δ x = substrate measured pO2 [bar] measured T [°C] measured R [Ω cm2] calculated R 600 °C, 0.21 bar pO2 [Ω cm2] here Macro 5 × 5 mm2 + CC↓ 0.4 LSGM 4 × 10–5 600 1 4 × 10–3* here Macro 5 × 5 mm2 + CC↓ 0.4 YSZ 4 × 10–5 600 2 9 × 10–3* ref 19 Macro 5 × 5 mm2 0.4 YSZ 1 × 10–3 400 120 2 × 10–2* ref 21 Macro 5 × 5 mm2 0.4 GDC/YSZ 4 × 10–5 450 254 2 × 10–1* ref 13 Macro 5 × 5 mm2 + 15 h annealed 0.4 YSZ 0.21 syn. air 600 5 × 10–1 5 × 10–1 42 × 10–1 42 × 10–1 ref 19 Macro 5 × 5 mm2 + 15 h annealed 0.4 YSZ 0.21 syn. air 600 6 × 10–1 6 × 10–1 46 × 10–1 46·× 10–1 ref 17 Macro 5 × 5 mm2 + 72 h annealed 0.4 YSZ 0.21 air 600 7 × 10–1 7 × 10–1 170 × 10–1 170·× 10–1 ref 22 Micro ø 0.2 mm 0.4 YSZ 0.21 air 550 2.5 9 × 10–1 ref 28 Micro ø 0.2 mm 0.4 YSZ 0.21 air 400 200 1.2 ref 24 Macro ø 5 mm 0.5 YSZ 0.1 600 5 3.1 ref 23 Micro ø 0.2 mm 0.2 GDC/YSZ 0.1 520 50.5 5.5 ref 26 Micro ø 0.2 mm 0.4 GDC/YSZ 0.1 520 55 6 ref 27 Macro ø 10 mm 0.4 GDC Pellet 0.21 syn. air 725 1.5 13 ref 20 Macro 10 × 10 mm2 + CC↑ + 45 h annealed 0.2 GDC/YSZ 0.21 air 530 82 18 1860 412 ref 31 Macro 10 × 10 mm2 + CC↑ 0.2 GDC/YSZ 0.21 air 550 65 23 ref 30 Micro ø 0.2 mm 0.2 GDC/YSZ 0.1 510 700 60 ref 25 Micro ø 0.06 – 0.1 mm 0.4 YSZ 0.21 air 750 7 88 ref 32 Micro ø 0.2 mm + 67 h annealed 0.2 GDC/YSZ 0.1 550 424 93 20977 7337 ref 29 Macro ø 17 mm 0.4 GDC Pellet 0.1 800 45 712 aThe term “Macro” refers to LSC thin films that were directly measured after PLD processing without current collecting thin film grid or with current collector beneath (CC↓) or after application of a thin film current collector on top (CC↑).", "“Micro” refers to electrode thin films, which underwent a micro-structuring step after thin film preparation.", "Some references include ex situ measurements of freshly prepared samples and values after annealing for given times.", "Asterisk (*) indicates that the pressure during measurement was much lower than 0.21 bar and thus extrapolation includes more uncertainty.", "For the sake of comparison, Table 2 also includes Rsurf,exch values of several LSC thin films deliberately degraded by annealing.", "An increase by 1–2 orders of magnitude already after several 10 h was found by different authors.", "The degradation mechanism of LSC is not fully understood yet but there is general agreement that strontium surface segregation plays a major role.17,18,20,62 Recently, it was also found that very small changes of the LSC surface, by depositing fractions of atomic layers of different oxides on the surface, can severely change the oxygen exchange kinetics.21 The large scatter of Rsurfexch values measured on supposedly freshly deposited LSC thin films might therefore only reflect different surface states obtained unintentionally because of (i) preparation procedures, films grown on polycrystalline or single crystalline substrates, with or without GDC buffer layers, PLD conditions (temperature, p(O2), laser fluence, substrate-target distance, cooling procedure), sample cleaning by solvents, current collector preparation on top or below, microstructuring; (ii) sample storage conditions, humidity, gas composition (e.g., with CO2, S-containing gases), storage time; and (iii) setup for electrochemical measurements, heating procedure, purity of applied gas mixtures, possible contamination sources inside setup (including Si), temperature gradients during microelectrode measurements.", "Any of these steps might alter the surface or even the microstructure of the LSC thin film and thereby its oxygen exchange kinetics.", "Owing to the multiple parameters involved from preparation to electrochemical characterization, which not only differ between studies but are often not deliberately chosen or unknown, it is not possible to explain the scatter of Rsurfexch by a single parameter.", "Still, two general conclusions can be drawn from the studies presented in Table 1.", "First, avoiding additional preparation steps after thin film deposition, that is, microstructuring, current collector preparation on top, or any other steps that might risk contamination of the surface by carbon residuals, Cr or Si poisoning, SO2 and CO2, has a positive effect on the oxygen exchange kinetics.63−66 Second, two ex situ studies and this in situ study (asterisks Table 1), report extraordinary low values for the (normalized) oxygen surface exchange resistance.", "These films do not differ in their PLD preparation parameters (and thus crystal structure) from others with much higher surface exchange resistances.13,19 However, these samples with very active surfaces have in common that the LSC thin films were never subjected to p(O2) above 10–3 bar at elevated temperatures in contrast to the other films of Table 2.", "Differences of the oxygen exchange kinetics between ref (21) and this study, both measuring impedance inside the PLD, probably arise from the fact that the LSC thin film in ref (21) was prepared, cooled down, stored outside, remounted in the PLD and then heated to the measuring temperature.", "Further, ref (19) shows only a comparatively slow degradation with an Rsurfexch increase by a factor of 2 after annealing 16 h at 400 °C in 10–3 bar p(O2) and in the Supporting Information of ref (21) even absence of any degradation was found for a thin film annealed at 450 °C for 7 h in 4 × 10–5 bar p(O2).", "Although in this study (600 °C, 4 × 10–5 bar p(O2)) degradation was not deliberately measured, since further LSC was deposited every 15–30 min on top of the existing layers, it should be noted that no evidence of any degradation was found during these intervals.", "Therefore, a low p(O2) seems to be advantageous for realizing highly reproducible measurements without any noticeable degradation.", "Mechanistic reasons behind both high catalytic activity and slow or nonexisting degradation at low p(O2) are unknown yet and a detailed understanding requires extensive further studies.", "However, they might be a consequence of stabilizing a less Sr-enriched LSC surface in mildly oxidizing environment.", "Lee et al.67 found for Ca, Sr and Ba doped LaMnO3 that higher oxygen partial pressures, 1 versus 1.3 × 10–9 bar p(O2), lead to dopant surface segregation and even formation of secondary phases above 500 °C.", "In accordance with this, Tselev et al.68 deposited La5/8Ca3/8MnO3 thin films using PLD at 6.7 × 10–5 and 2.7 × 10–5 bar p(O2) and discovered that the surface changed from an almost complete A-site termination to almost exclusive B-site termination, respectively.", "Owing to a possible change of a freshly prepared surface when increasing p(O2), it is also somewhat questionable whether the oxygen partial pressure dependence used for normalization (i.e., m = 0.63 used here) also applies to these highly active LSC thin films.", "The calculated surface exchange resistance in the last column of Table 1 may thus underestimate the true resistance in air.", "Further investigations of the oxygen partial pressure dependence inside the IPLD setup have to at which stage LSC surfaces lose parts of their high catalytic activity and in combination with chemical analysis might reveal key processes of performance changes.", "Conclusions A novel method is introduced to characterize the electrochemical properties of freshly prepared as well as growing MIEC thin film electrodes by in situ impedance spectroscopy during pulsed laser deposition.", "Thin film growth and electrochemical characterization of LSC thin film electrodes are performed simultaneously, that is, under the same conditions, and this allows to monitor kinetic and thermodynamic film properties also for early stages of film growth.", "On the basis of a simplified equivalent circuit the electrochemical film properties (oxygen surface exchange resistance, chemical and interfacial capacitance) can be successfully extracted.", "The metallic current collector grid, prepared on top of the electrolyte prior to film deposition to ensure homogeneous film polarization, affects the oxygen exchange only in the very beginning of LSC film growth (up to 3 nm LSC).", "However, during the first 20 nm of LSC growth, a decreasing electronic sheet resistance still limits the active electrode area to parts close to the current collector grid.", "Above a film thickness of 20 nm, a thickness independent oxygen surface exchange resistance of 2.04 ± 0.1 Ωcm2 is obtained at 600 °C and 40 μbar O2 for LSC grown on YSZ.", "The thickness dependence of the electrode capacitance indicates an interfacial contribution of 1012 ± 253 μF/cm2 and a thickness independent volumetric chemical capacitance of 1281 ± 39 F/cm3.", "The reproducibility of these values was very high, that is, relative errors are unusually low.", "These experiments thus allow determining the electrochemical properties of freshly prepared MIEC films before exposure to any change of temperature or gas atmosphere.", "The measured oxygen exchange resistance of such freshly prepared LSC surfaces is impressively low, taking into account that it refers to an oxygen partial pressure 5000 times smaller than in ambient air.", "A literature review of polarization resistance of LSC films revealed tremendous scatter, but also showed that in usual ex situ measurements most LSC films did not reach such a low polarization resistance even for oxygen partial pressures as high as 0.2 bar.", "Freshly prepared LSC films never exposed to temperatures, oxygen partial pressures and gases other than those used during deposition thus seem to be electrochemically extremely active.", "The excellent reproducibility of the measurements also allowed investigation of the influence of comparatively small lattice mismatch (∼0.3% at 600 °C) in LSC thin films grown on LSGM single crystals.", "An enhancement of the oxygen exchange kinetics by a factor of 2 was found for strained LSC films on LSGM compared to unstrained films on YSZ.", "Moreover, a higher chemical capacitance of 2033 ± 21 F/cm3 was obtained, suggesting a decrease of the oxygen vacancy formation energy for tensile strained MIEC thin films leading to higher oxygen vacancy concentrations.", "Supporting Information Available The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acsaem.8b00586.", "Microscope and AFM images of the MIEC samples, details on temperature measurement and temperature control during IPLD experiments, estimate of the decay length of electrochemical activity, and impedance spectra of LSC films grown on LSGM (PDF) Supplementary Material ae8b00586_si_001.pdf The authors declare no competing financial interest." ]

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