bluuebunny/crossref_metadata_2025_split huggingface dataset:
Innovative Processes for a Low Impact in the Electroplating of Stainless Steel
Authors: Giurlani Walter , Biffoli Fabio , Pappaianni Giulio , Mariani Elena , Meoli Arianna , Dini Tommaso , Pizzetti Federico , Innocenti Massimo 
Published: November 2022

Steel is a cheap renewable material with many interesting properties but its presence in the electroplating sector is very limited due to adhesion difficulties. Stainless steel contains approximately 10.5% chromium, which forms a surface oxide layer that passivates the steel, making it resistant to corrosion [1]. It is the presence of this surface oxide film that makes it difficult to electroplate steel. The aim of electroplating steel is to refine it by depositing nobler metals of the desired color, such as ruthenium and gold.
The activation of steel involves the remotion of the oxide layer. The main method of electroplating stainless steel is generally through the deposition of nickel, but the intensive use of nickel baths makes these processes inappropriate for the sustainability paths taken by the electroplating industry. Even when nickel-based galvanizing processes are not used, it is possible that steel objects do not pass the nickel release test. This is because the steel itself contains nickel, so the removal of the surface oxide layer during the electroplating process may facilitate the release of nickel.
The nickel release mechanism is not yet fully clear but bring to allergenic issues in the final product [2]. We performed a systematic study electroplating various metals and alloys on steel to evaluate which one performed better as barrier against the release of nickel and shed light on this issue.
The steel substrate was characterized microscopically and spectroscopically before and after the release test. The amount of nickel was evaluated in the solution that simulates human sweat to evaluate its release in µm·cm-2·week-1 according to the standard EN 1811:2015.
The authors acknowledge Regione Toscana POR CreO FESR 2014-2020 – azione 1.1.5 sub-azione a1 – Bando 1 “Progetti Strategici di ricerca e sviluppo” which made possible the projects “A.C.A.L. 4.0” (CUP 3553.04032020.158000165_1385), “A.M.P.E.R.E.” (CUP 3553.04032020.158000223_1538), “GIGA 4.0” (CUP 3553.04032020.158000105_1242) and “GoodGalv” (3647.04032020.157000060).

References

[1] Olsson, C. O. A.; Landolt, D. Passive films on stainless steels—chemistry, structure and growth. Electrochim. Acta. 2003, 48, 1093-1104, doi:10.1016/S0013-4686(02)00841-1.
[2] Yuan, J.P.; Li, W.; Wang, C.; Ma, C.Y.; Chen, L.X.; Chen, D.D. Nickel release rate of several nickel-containing stainless steels for jewelries. J. Iron Steel Res. Int.
2015, 22, 72-77, doi: 10.1016/S1006-706X(15)60012-7.
Insights and Applications of Composite Electroplating
Authors: Fransaer Jan 
Published: November 2022

Composite electroplating is the process of particle incorporation during the electrolytic deposition of metal. This process produces composite films consisting of a metallic matrix containing a dispersion of small particles. The advantages of composite electrodeposition over other coating methods are the uniformity of deposition even for complex shapes, the strong adhesion to the substrate, reduction of waste compared to dipping or spraying techniques, low levels of contamination, the ability to produce functionally-gradient material and to continuously process parts. In addition, this process avoids the problems associated with high temperature or vacuum processing.
There are many contradictory experimental results in literature concerning the effects of the electrocodeposition process variables on particle incorporation. The effects of some of the process variables also vary for different particle-electrolyte combinations and cell configurations. Some of the reported contradictions are a direct consequence of incomparable hydrodynamics. The bulk of experimental electrocodeposition research has been conducted using a vertical parallel plate electrode set-up. In this configuration, the particles are maintained in suspension by either stirring the solution, vibrating a perforated plate at the bottom of the cell, bubbling gas, or pumping the suspension through the cell, all of which result in uncontrollable, and hence incomparable hydrodynamics. Other contradictions are due to the fact that the process parameters were evaluated only for a narrow range of experimental parameters and to differences in particle size and purity.
This talk discusses the experimental results and mathematical modeling of electrocodeposition of particles in a metallic matrix. The effects of several key parameters, such as current density, particle loading, electrolyte composition, particle surface charge and polarity, on particle incorporation in electrodeposited composite coatings were studied and modeled. All experiments were done utilizing rotating disk electrodes over a wide range of experimental conditions in which the incorporation behavior changes appreciably, yielding reproducible data for better interpretation of process effects and modeling. These studies were combined with colloidal probe AFM experiments and process archeology using pulse plating which helped to understand the codeposition mechanism.
(Digital Presentation) Electrochemical Conversion of Cu Nanowires Synthesized By Electrodeposition in Track-Etched Templates to HKUST-1
Authors: Luo Jia , Wagner Michael Florian Peter , Ulrich Nils , Kopold Peter , Trautmann Christina , Toimil Molares Maria Eugenia 
Published: November 2022

Metal-organic frameworks (MOFs) are a novel type of nanoporous materials that have attracted widespread attention over the past two decades [1]. Cu-based metal-organic frameworks such as Cu3(BTC)2 (also known as HKUST-1) are one of the most famous MOF representatives, which exhibit a huge open porosity and thus a remarkably capacity to store and uptake different gases [2, 3]. Recently, increasing efforts are devoted toward finding synthetic routes that enable downsizing MOF crystals to the nanoscale. Achieving control over the size and shape of nanoMOFs and finding ways to assemble them is essential for their exploitation in integrated devices such as sensors, gas separation membranes or photoelectrodes.
In this study we explore the conversion of free-standing arrays Cu nanowires with controlled diameter and length synthesized by electrodeposition in etched ion-track membranes into HKUST-1. In a first process step, free-standing Cu wires are produced by dissolving the ion-track polymer template. In a second step, the wires are converted into HKUST-1 structures by electrochemical oxidation. Applying 2.5 V versus a Cu counter electrode, the Cu nanowires are oxidatively dissolved and the MOF is built up as the as-formed Cu2+ ions bind to the BTC3− ligands in the electrolyte solution. The morphology and crystallinity of the samples at different transformation stages is investigated by scanning electron microscopy (Fig. 1) and transmission electron microscopy, respectively. X-ray diffraction spectra measured at different conversion times reveal the appearance of the characteristic reflections of HKUST-1. These results will be compared with previous studies of the transformation of Cu nanowires to HKUST-1 nanowires inside the polymer membrane [4].
Figure 1: SEM images of cylindrical Cu nanowires (a) before and (b) during the electrochemical conversion process, and (c) of a representative octahedral particle after complete conversion to HKUST-1.

References

[1] Freund R, Canossa S, Cohen SM, Yan W, Deng et al. Angewandte Chemie International Edition. (2021) 2: 23946-23974
[2] Chui SS-Y, Lo SM-F, Charmant JP, Orpen AG, Williams ID. Science. (1999) 283:1148-50.
[3] Li H, Li L, Lin R-B, Zhou W, Zhang Z, Xiang S, et al. EnergyChem. (2019) 1:100006.
[4] Caddeo F, Vogt R, Weil D, Sigle W, Toimil-Molares ME, Maijenburg AW. ACS applied materials & interfaces . (2019)11:25378-87.

Figure 1
Fabrication of Electroplated FeCo Nanowires in AAO Substrate for the Application to Inductor
Authors: Kim Dong Hyun , Kim In Yea , Lim Gi hwan , Kim Chae Yoon , Lee Min-Jeong , Kim Jaehun , Lim Jae-Hong 
Published: November 2022

Recently, demand for inductors is increasing due to the development of IoT, automatic driving devices, and eco-friendly electric vehicles, and for this reason, efficient and miniaturized inductor manufacturing technology is becoming important. To miniaturize the inductor, it is necessary to miniaturize the core part, which is the center of the inductor. A typical method for manufacturing a core part of inductor is a multilayer ceramic capacitor (MLCC). This method cross-laminate silicon and metal in order to make patterns. After cross-laminating, it needs to be contracted to make it smaller in sintering process. This process causes imprecision of dimension thus there is a limitation in miniaturization of the inductor.
The diameter of AAO used in this study is 25mm and its pore size is 200nm. 3 electrode electroplating is selected for plating FeCo on AAO, counter elctrode as Pt electrode, and FeCo were deposited on –1 V vs. Ag/AgCl and on differed time for 6h, 7h, and 8h. The concentration of electrolytes used for FeCo plating is Fe 0.15 M/L, Co 0.2 M/L, and ascobic acid 0.01 M/L. For electrolytes, 47.4 g/L of cobalt chloride hexahydrate, 35.6 g/L of ion sulfate hepahydrate, and 1.769 g/L of L - ascobic acid were used. After the plating, SEM images and EDS were used to see the deposition rate of FeCo nanowires and composition variation via time.
FeCo nanowires were generated via time for 6h, 7h, and 8h to see the deposition rate. Figure 1 shows SEM image of FeCo nanowire plated for 8 hours and figure 2 shows length of the FeCo nanowire via time. After removing the AAO using 3M NaOH, we measured the saturation magnetization of FeCo nanowire and was 167.2269 emu/g and the coercivity was 120 Oe as shown in figure 3. The saturation magnetization was different from theoretical value of FeCo, 245 emu/g, probably due to the poor crystallinity. The more details will be presented.

Figure 1
Electrodeposition of Functionally Graded Brazing Interlayers for Enhanced Joint Strength between Fusion Plasma-Facing Materials and Heat Sinks
Authors: Lee Katherine , Garich Holly , Snyder Stephen , Skinn Brian , Inman Maria 
Published: November 2022

In response to the significant plasma science and engineering breakthroughs witnessed over the past decade, the fusion research community has developed an ambitious roadmap to achieve large-scale, energy-positive fusion reactors that will enable economically competitive fusion electricity. Critical to the success of commercial fusion energy is the development of materials able to serve as plasma facing components (PFCs) that can withstand the unprecedented high heat, particle, and neutron fluxes within the fusion reactor. Tungsten is a leading candidate for the plasma-facing portion of these PFCs because of its high melting point, high sputtering resistance, and low tritium retention. Copper or copper-based alloys (e.g., copper-chromium-zirconium alloy C18150) and reduced activation ferritic/martensitic (RAFM) steels have been proposed for the heat sink materials behind the tungsten armor due to their high thermal conductivity. Brazing is considered a promising method for joining the tungsten armor and heat sink layer. However, the extreme mismatch in the coefficient of thermal expansion (CTE) between tungsten and these potential heat sink materials makes directly joining these two layers challenging. This thermal stress can be reduced by incorporating a joining layer of functionally graded materials between the tungsten and heat sink that imparts gradual changes in CTE. Copper/tungsten or copper/tungsten carbide composites are leading candidates for these functionally graded materials. For these composites, gradual changes in the CTE are achieved by varying the volume fraction of tungsten/tungsten carbide in the composite, from tungsten-rich at the tungsten armor to tungsten-poor at the heat sink.
This talk will discuss the development of a scalable, electrochemical approach for fabricating interlayers with functionally graded CTE that can decrease the thermal mismatch between tungsten PFCs and copper or RAFM-based heat sinks. In this approach, the copper/tungsten or copper/tungsten carbide composite are electrodeposited onto the tungsten PFC. This component is then bonded to the heat sink via brazing. A key objective of the work is to achieve compositional control during electrodeposition through the use of highly tunable pulse and pulse-reverse electric fields. Engineering of the electric field enables control of the mass transport and crystallization phenomena in the deposition process and thus enables control of composite properties such as composition, porosity, and surface roughness. Results from electrodeposition trials and mechanical testing of brazed joints under ambient conditions as an initial screen for interlayer performance will be discussed, in anticipation of high-heat flux testing of joint performance under fusion-relevant conditions.
Perspectives and Impact of in-Situ X-Ray Techniques for Electrodeposition
Authors: Grunder Yvonne 
Published: November 2022

In-situ surface x-ray diffraction has enabled an atomic/molecular-level understanding of the electrochemical interface, including its potential and time dependence, to be developed. [1] Specifically, for electrodeposition the influence of additives and adsorbates onto growth and nucleation behaviour could be established. Halogens on metal surfaces are prototypic adsorbate systems but the adsorption of halide ions especially on copper is also of major importance for on-chip metallization in ULSI microchip production. Halide ions on Cu surfaces form an inhibiting adsorbate layer with polyethylene glycol (PEG). Even though the influence of the additives combination on the shape evolution of the Cu deposit was subject of numerous studies, their precise role during the elementary steps of the deposition with regards to altering the charge distribution and dipole moment at the interface is largely not understood. [1] While information about the atomic structure of the electrode surface in electrochemical in-situ cells has been widely investigated, insight into the charge distribution and the structure of the electrolyte at the interface is still lacking. Combining x-ray spectroscopy and x-ray diffraction to gain site-specific information about the charge distribution at buried interfaces is a promising tool. [2,3,4]
Studies on the metal-halide interface and how the use of surface x-ray scattering techniques can help to characterise electrochemical interfaces in-situ in order to link, structure and stability and morphology changes will be presented. [1, 4] Advances in these directions offer possibilities in elucidating atomic scale models of the electrochemical interface and thus will help to establish structure-stability-reactivity relationships which will help to understand growth kinetics and nucleation behaviour.

References:

[1] In-Situ Surface X-ray Diffraction Studies of Copper Electrodes: Atomic-Scale Interface Structure and Growth Behavior. Gruender, Y., Stettner, J., & Magnussen, O. M. (2018). Journal of the Electrochemical Society; 166(1), D3049-D3057. doi:10.1149/2.0071901jes

[2] Probing the charge distribution at the electrochemical interface; Y. Gründer and C. A. Lucas, Physical Chemistry Chemical Physics, 2017, 19, 8416
[3] Simulation of Surface Resonant X-ray Diffraction; Y. Joly et al., J. Chem. Theory Comput,. 2018, 14, 973−980
[4] Charge Reorganization at the Adsorbate Covered Electrode Surface Probed through in Situ Resonant X-ray Diffraction Combined with ab Initio Modeling;Y. Grunder, C. A. Lucas, P. B. J. Thompson, Y. Joly, Y. Soldo-OlivierJ. Phys. Chem. C 2022, 126, 9, 4612–4619
Challenges in Understanding Electrochemical Growth
Authors: Magnussen Olaf M. 
Published: November 2022

Over the past 100 years, electrodeposition has matured to an important method with numerous industrial applications, up to processes in micro- and nanofabrication. Knowledge on electrochemical processes on the atomic scale is still limited, however. While for vapor deposition under vacuum conditions the evolution of the deposit morphology can nowadays be predicted with high precision, a similar predictive understanding of electrodeposition is missing so far. A key issue here is the electrochemical interface where this growth occurs. The structural complexity of this interface on the one hand makes understanding of the elemental processes in nucleation and growth difficult. On the other hand, it is just this complexity that allows to tune electrodeposition processes in ways that are not possible for deposition in vacuum and thus make them attractive for many applications.
In this talk, I will discuss current challenges in developing a true microscopic picture of electrodeposition processes, using examples from us and other groups. The focus will be on puzzling experimental observations and fundamental aspects that we do not yet understand and thus provide a rich field for future research. These include the mechanisms of elemental steps in electrochemical growth processes, such as ion transfer, intra- and interlayer surface diffusion, and the resulting development of the deposit morphology. Of particular interest is how these events are influenced by the electric field and electrolyte species in the electrochemical double layer, which is of key relevance for understanding the effects of overpotential and additives. A further challenge is to extend the insights obtained for electrodeposition of metals to the electrochemical growth of compound materials, such as oxides.
Examples, Perspectives, and Impact of in-Operando Electrochemistry & Electrodeposition
Authors: Rost Marcel J. 
Published: November 2022

In order to leave our children not with a huge problem in the future, we quickly have to realize the energy transition to renewable and CO2 neutral sources and circuits, which implies the introduction of the complete H2 economy. In addition, the ever ongoing demand and progress in electronics requires new and smart steps from the semiconducting industry pushing the border for device fabrication and thus material science and nanotechnology.
Both extremely important topics crucially depend on the complete understanding of the fundamental atomic processes for device or catalyst manufacturing by electrodeposition as well as their stability during operation under (electrochemical) application.
The general problem, however, has been formulated nicely already by Wolfgang Pauli:
„God made the bulk; surfaces were invented by the devil.“
It took around two decades, before most of the basic concepts and atomic effects have been observed and understood in standard, ultra-high vacuum (UHV) surface science and nanotechnology. Now, it is surely time to open a similar book and start from scratch, as atoms and surfaces in electrochemical environment clearly behave differently than in UHV. Moreover, this time it is not enough to measure after the deposition, after the growth, after the nucleation, or after a reaction!
Both electrochemical data clearly show that many surfaces change during application and the complex understanding during electrodepostion, which involves a huge parameter space of tunable variables, can surely only be addressed adequately by in operando measurements.
In this talk, I will show examples from in operando measurements ranging from STM over TEM to SXRD and X-ray photoelectron spectroscopy that all demonstrate the power and perspective for gaining new insight.

Figure 1
(Digital Presentation) Electrodeposition of Free-Standing Porous Cu Frameworks for Energy Applications
Authors: Kurniawan Mario , Calmbach Jasmin , Zullufi Kosovare , Stich Michael , Bund Andreas 
Published: November 2022

Recently, a convenient method has been suggested to produce a highly porous metal structure such as Cu using a single-step electrodeposition method [1]. In this approach, hydrogen bubbles are used as dynamic templates during the metal electrodeposition process to create the micro-porous structure. However, the pore walls of the porous layers often grow in ramified dendritic structure, which results in limited mechanical stability and creates challenged for applications in compact devices.
In this contribution, a novel approach will be discussed to improve the mechanical stability of these porous structures by employing a second electrodeposition step. This process greatly reduces the number of dendrites within the pore walls making the porous layer more compact and thus improving the mechanical stability significantly. Furthermore, a complete separation of the porous layer from the flat substrate can be achieved by ultrasonication to obtain a free-standing porous Cu framework. Some parameters such as the layer thicknesses and pore sizes can be tuned easily by changing the current density and the electrodeposition time, respectively.
The use of thus prepared free-standing porous Cu frameworks will be discussed for photoelectrochemical (PEC) water splitting and CO2 reduction. For the PEC water splitting application, a photoactive Cu2O layer is electrodeposited on the free-standing porous Cu framework. A homogenous coating of the Cu2O can be achieved and the PEC performance shows a significant increase of photocurrents by more than 80 % at 0 V vs. RHE in comparison to the Cu2O planar substrate [2]. For the CO2 reduction application, a large sample with10 cm2 geometric surface area was successfully prepared. The sample was used in a custom-made electrochemical cell with a cation exchange membrane as a separator. CO2 gas in a high humidity environment is transported to the free-standing porous Cu working electrode via a membrane pump in a closed-loop system. Our preliminary results show formation of ethylene and ethane gas using gas chromatography which indicates a successful reduction reaction of the CO2.
[1] H.C. Shin., M. Liu. Chem Mater 16:5460–5464 2004. Doi:10.1021/cm048887b
[2] M. Kurniawan, M. Stich, M. Marimon, M. Camargo, R. Peipmann, T. Hannappel, A. Bund, J. Mater. Sci.
2021, Doi:10.1007/s10853-021-06058-y
A Room Temperature Electrodeposition Method to Develop High Performance Metal-Chalcogenide Nanowire Array-Based Photoelectrochemical (PEC) Device for Solar Hydrogen Production
Authors: Vijay Shiljashree , Cheng Wei , Jawahar Hussaini Syed Mubeen 
Published: November 2022

Photoelectrochemical (PEC) water splitting has emerged as a significant and promising technique for the generation of low-cost, highly efficient, and sustainable hydrogen(H2) fuel. Currently, PEC hydrogen production has been successfully demonstrated on a laboratory scale. However, the commercial viability of PECs depends critically on the cost of H2 produced by the PECs, which is affected by the cost of PEC construction. Here we consider electrodeposition as a promising method to fabricate multijunction PEC cells because this is an inexpensive solvent-based technique operated at low temperature with the ability to control the film thickness by varying the deposition potential and charge passed which can be optimized to perform like other matured and expensive vapor-based deposition techniques functioning at high temperatures.
In this research work, we report a room temperature, low-cost electrodeposition method to synthesize metal chalcogenide semiconductor thin films and nanowire arrays in superstrate configuration and demonstrate its applicability for solar hydrogen production. Specifically, the talk will address the effect of electrodeposition parameters and post-treatment on observed photocurrent and photovoltage responses. By optimizing the deposition potential and deposition charge we were able to achieve photocurrent densities exceeding 15 mA cm-2 for thin films and nanowire arrays when tested using regenerative redox couples.
Finally, the talk will cover the aspects of developing a buried junction PV/PEC using electrodeposited chalcogenide semiconductors for solar hydrogen production.