Chunxi
Hai, Takashi Shirai, Masayoshi Fuji, Chika Takai
先進セラミックス研究センター年報 (2012). Vol.
1, 35-43

解説

Developing Applications of Electrically Conductive Alumina with in Situ
Nano-carbon Networks (NCN)
Chunxi Hai, Takashi Shirai, Masayoshi Fuji, Chika Takai
Advanced Ceramics Research Center, Nagoya Institute of Technology,
3-101-1 Honmachi, Tajimi, Gifu 507-0033, JAPANElectrically conductive alumina (CA) with two forms conductive dense alumina (CDA) and conductive porous alumina (CPA)
fabricated by combination of gelcasting and high temperature reductive sintering (HTRS) was claimed to a novel functional
material with high-performance. With the aid of HTRS, polymer networks were thoroughly converted to carbon with graphitic
structure. Taking the unique structure of CA into consideration, it is no suspicious that CA is available as electro-catalyst andmicrowave-induced heater. Herein, in this study, several modification methods have been designed in order to get the enhanced
performances.

1. INTRODUCTION

Electrically conductive ceramic (CC) has been one of
the research points recently determined by its various
advantages. These merits involve physic-chemical andthermal stability, high erosion resistivity, low cost etc. [15] So far, either conductive matrices or additives havebeen employed to get CC via different preparing
methods. These methods involve hot press [6], spark
plasma [7], sol-gel [8] etc. However, it is still difficult tomake uniformly dispersed conductive networks in Al2O3
matrix [9-20]. Various carbon additives are facilitated toagglomerate in composite, thereby leading to thesegregated conductive phase and weak bending strength.

Thus, that is certainly necessary to explore a newprocess that not only is simple and direct method, butalso provides homogeneously dispersed conductive
networks. Herein, a new era has been developed since
the initial announce of conductive alumina (CA) which
was fabricated by combination of gelcasting and hightemperature reductive sintering (HTRS) [21-24]. In thismaterial, it was confirmed that the uniformly dispersed
carbon with graphitic structure attributes to the goodelectrical conductivity of CA. With the aid of
mechanically forming by hand-mixer at the highest
speed, conductive porous alumina (CPA) with highporosity up to 66.23% was also fabricated in our study.

Fig. 1. Schematic of preparing conductive alumina (CA)[21-24]― 35 ―

Developing Applications of Electrically Conductive Alumina with in Situ Nano-carbon Networks (NCN)

Fig. 2. TEM images of CA[21] (a), (b) and (c) and Raman spectroscopy of CA (d)[28]

Fig. 3. Schematic illustration between densifying and coarsening procedures micro-structure changes of CA via high temperature
reductive sintering (HTRS) resulting graphitization of polymer networks

Fig. 4. (a) Schematic diagram of relationship between electrical conductivity and thermal conductivity of CA, (b) Photograph of CA
electrical conductivity and (c) Temperature-time curves of CA for liquid paraffin via microwave irradiation

Therefore, there are two forms for CA, namely
conductive dense alumina (CDA) and conductive porousalumina (CPA).
Taking the unique structure of CDA and CPA into
consideration [21-24], it is reasonable that various
potential applications are designed as shown as follows.
Because of the good conductivity, structure and property
stability, microwave irradiation induced increased

temperature of CA was confirmed and various
modification ways had been completed. Besides theabove suppose, due to the electrical conductivity of CA
and high accessible surface area, a novel electro-catalyst
employing CPA was also constructed.
2. MICROWAVE-INDUCED HEAT PER-FORMANCE― 36 ―

Conductive

alumina(CA)

wasfabricatedbyChunxi Hai, Takashi Shirai, Masayoshi Fuji, Chika Takai

combination of gel-casting and HTRS in Ar [21-24].
With the aid of HTRS, the polymer networks formed ingel-casting technology were totally converted to nanocarbon networks (NCN), thereby leaving the electricalconductivity of ceramic. The preparing process is
proposed in Fig. 1.
Nano-carbon and alumina grains co-exist together asshown in Fig. 2 (a), (b) and (c). More, Raman spectrum
also confirms the electronic crystal structure of carbon
is graphitic as displayed in Fig. 2 (d) [25-28].
It is noticed that HTRS attributes to the completed
conversation of carbon from well gelled polymer
networks, thereby forming the nano-graphitic carbon

crosslinks in CA.
Then, it is reasonable to conclude that grapheneorientation can be controlled by HTRS.
HTRS effect on graphitic orientation is supposed inFig. 3. As the increased temperature, polymer is initiallyconverted to amorphous carbon followed by accelerating
to graphitic structure. Higher temperature benefits to theimproved graphitic orientation, which is verified by thedecreased surface defects calculated from Raman
spectroscopy
analysis(RID/IG (CDA-1400°C)=1.26>RID/IG (CDA-1700 °C)=0.35) [21].
Furthermore, besides the good electrical conductivity(Fig. 4 (b)), both CDA and CPA have microwave

Fig. 5. (I) Flow-chat of CNT/CPA[30], (II) Change of CNT by pre-treating[29] and (III) FE-SEM images of CNT/CPA[30]― 37 ―

Developing Applications of Electrically Conductive Alumina with in Situ Nano-carbon Networks (NCN)

Fig. 6. Schematic of Pt nanoparticles deposition via different heating methods (EG: Ethylene glycol)

absorbability, which benefits from the graphitic
networks in them, which could be confirmed by theincreased temperature of detected sample as shown in
Fig. 4 (c).
Generally, graphitic structure results in not only
conductivity,
but
also
electromagnetic
wave
absorbability. It is noticed that various properties of CA
results from graphitic structure of carbon. Taking thesimilar graphitic structure of carbon nanotubes (CNT)
into consideration, CNT/CPA was developed. The
corresponding experimental flow-chat and microstructure of CNT/CPA is shown in Fig. 5 (I) and (III),
respectively [29-30].
It is noticed that additive CNT was uniformly
dispersed in matrix as shown in Fig. 5 (III), which merits
from the surface pre-treatment by concentrated acids [2930]. CNT co-exist with NCN and alumina forming
ternary composite. Comparing with other CNT-based
composites prepared by hot press [25], spark plasma [7],sol-gel [26-27, 31] etc., CNT is more uniformly
dispersed in ceramic matrix. More, as introduced by
Mao et al. [32], microwave absorbability is not only
related with electron but also phonon. The increased
phonon intensity induced by CNT in composites
attributes to this performance. More, Vázquez et al. [20]have reported that CNT with higher impurities owns
stronger absorptions than ‘perfect’ one benefiting from
impurities-induced localized superheating and heating
performance of CNT is little related with its length.

Generally, the intensified phonon accelerates theincreased D intensity leaving the higher heating
performances [33].
Furthermore, Wei et al. [34] has claimed that match ofabsorbers plays an important role for accelerating theelectromagnetic wave absorbability and developing
various potential applications in many fields. To date,kinds of ferrite/dielectric (Fe3Al/Al2O3, YBa2Cu3O7FCC-Co/Al2O3,
Al2O3-coated
FeCo,
x/Al2O3,
BA0.65Sr0.65TiO3, (ZnMg) TiO3) have been reported [3439]. It was proven by Suttisawat et al., Pt nanoparticles
with uniform distribution was not only catalyst but also
good absorbent [40-41]. More, CA also has goodheating performance at the irradiation of microwave.
Herein, it is possible to design another composite byanchoring Pt nanoparticles via chemical reductive
reaction employing CA as substrate. Two heating
methods have been conducted. One is conventional oilbath heating, another is microwave-assisted heating. The
fundamental experimental mechanism is proposed inFig. 6.
Benefiting from carbon polarization by microwave
radiation, high selective surface modification of porous
ceramic with large size was completed.
Structural modification by both employing CNT andsurface modification via Pt nanoparticles at the aid of
microwave-assisted heating chemical reductive reaction
attributed to the enhanced heat performances, which
also claimed the potential application of CA as non-

― 38 ―

Chunxi Hai, Takashi Shirai, Masayoshi Fuji, Chika Takai

Fig. 7. Schematic representation of preparing M/CPA (Pt/CPA and Ni/CPA) via chemical reductive reaction[46]touching heater. And the increased heat phenomena
results from the intensified phonon signals. Thisconclusion was valid by Raman spectroscopy.
3. ELECTROCHEMICAL PERFORMANCEEVALUATIONAs shown in Fig. 7, the schematic employed in thisexperiment was proposed. Briefly speaking, three steps
were involved for making CPA-based composites
M/CPA. (a) Surface pre-treating, by which various
surface defects on NCN with graphitic structure areavailable. These defects include five- or sevenmembered rings in the carbon networks instead ofnormal ring, sp3-hybridized defects (H or OH) andvacancies in the carbon lattice [27]. Pre-treating of CPA
attributes to increased sp3-hybridized defects (-COOH, -COH etc.) [42]. (b) Absorption of Mn+ onto substrate via
electrostatic interaction and (c) Chemical reduction of
Mn+ to M particles [46]. More, conventional threeelectrode evaluation system was constructed to evaluate
the electro-performances of different composites.
Using CPA as reference, it is confirmed thatfunctional particles have been successfully deposited
onto the surface of matrix by surface decoration (Fig. 8(a), (b) and (c)). Comparing with Ni/CPA composite, it
is noticed that Pt/CPA has higher selectivity. The electroperformances of as-resulted composites have been
evaluated in 1 M NaOH solution at the same
experimental condition. The enhanced performance ofpre-treated CPA is attributed to grafted functionalgroups by covalent modification [28]. As-received andpre-treated CPA display electro-catalytic activities

Fig. 8. FE-SEM images of (a) CPA, (b) Ni/CPA and (c) Pt/CPA and (d) Cyclic voltammetric (CV) curves of different electrodes
developed in this study[45-46]― 39 ―

Developing Applications of Electrically Conductive Alumina with in Situ Nano-carbon Networks (NCN)

toward oxygen reductive reaction (ORR), which can beproven by similar slopes of the reductive current withdecreasing potential from -0.3 V to -0.2 V. Moreover,
ORR occurred at potentials of -0.1 V~+0.4 V for Pt/CPA(Fig. 8. (d)). It is believed that the ORR activity of the
Pt/CPA at more positive potentials is attributed to Pt (5d orbital vacancies) nanoparticles deposition. And theenhanced performance of Pt/CPA can be verified by theincreased current and enlarged time window as shown in
Fig. 8 (d). Meng et al. [42] reported the ORR activity of
Pt/C at potentials of +0.7 V. Pt/CNT/CHIT was also
claimed to be ORR activity electro-catalysts at the samemeasurement condition and the ORR activity occurred
at +0.1 V. Then, by surface modification, it was
confirmed in this study that as-fabricated composites
have a potential application in fuel cells [43-46]. Basedon the features of substrate, different surface
modification schematics have been proposed in Fig. 6
and Fig. 7.
4. POTENTIAL APPLICATIONS OF CA WITH
MODIFICATIONS

Since good electrical conductivity, micro- structureand enhanced performances of CA via modifications,various attractive wide- spread potential applications
ranging from heater [1-5], decomposition [47] andtransfer hydrogenation (TH) process [48] etc. aredesignable. Subsequently, in this section, we will briefly
introduce the different application directions of CA as
shown in followings.
a. Non-contacting Heater Application
Even though microwave absorbents display intriguingcharacteristics in many fields [47-49], microwave
transparent materials are limited in this field. To date,
SiC was reported to good heaters by Kremsner et al. [50]Therefore, due to the graphitic carbon, CA and CAbased composites are available as non-contacting heaterfor microwave inert medium.
b. Decomposition and hydrogenation application
Pt/substrate composites combining the advantages ofmatrix and uniformly dispersed Pt nanoparticles permits
the possibility for organic decomposition at the aid ofdifferent method such as electrochemical evaluation[51], electromagnetic wave radiation [52] or ultra-highvacuum (UHV) [53] etc. More, according to the varied
reaction mechanisms, different reaction routes with highselectivity are accessible. Herein, because of the
microwave capacity of CA, TH or decomposition or
combination utilizing CA or Pt/CA as heater andcatalyst at the microwave radiation is reasonable.
c. Electro-catalyst application
Commonly, conductor and semi-conductor are
regarded as idea electrode materials as introduced inreferences [44,46,51,54-55]. Therefore, considering theelectrical conductivity of CA and related CA
composites, they are believed as electrode candidates
with high-performance. It is significant to explore anovel electro-catalyst by kinds of surface modification
for different practical applications.
5. CONCLUSIONSIn this review, characteristic, property and influence
factors of CA with two forms (dense (CDA) and porous(CPA)) have been demonstrated. Meriting fromconductivity and property stability of matrix, various
widespread potential applications are accessible for us.
In order to gain the improved performances ofcomposites, both structural and surface modifications
have been conducted. Eventually, as-prepared
composites can be designed as non-contacting heater,
decomposition, TH and electro-catalyst etc.
ACKNOWLEDGEMENT

This study was finically supported by Ministry of
Education, Culture, Sports, Science and Technology(MEXT), Project “Cooperation for Innovative
Technology and Advanced Research in Evolution Area”.
This work was also supported by The Hori Sciences andArts Foundation.

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