解説

先進セラミックス研究センター年報（2014）．Vol．3，5-10

Silicon Carbide and Its Nanostructures
Jin Li*, Takashi Shirai**, Masayoshi Fuji*** R&D Centre for Vehicle Battery and Energy Storage, General Research Institutefor Nonferrous Metals, Beijing, 100088, China** Advanced Ceramics Research Center, Nagoya Institute of Technology
3-101-1, Honmachi, Tajimi, Gifu 507-0033, Japan
E-mail address: fuji@nitech.ac.jp
Abstract
Silicon carbide (SiC) is a promising ceramic for various industrial applications thanks to its excellent properties at hightemperature, high power, high frequency, high radiation environment and chemically harsh conditions. Substantial efforts havebeen made to develop new approaches to the synthesis of SiC and its nanostructures. Nanostructured SiC including nanoparticles
and one-dimensional (1D) structures are superior to their bulk counterpart in many properties, and have attracted considerable
attention in recent years due to their important role in basic science and their potential applications in electronic and optoelectronic
devices, and composite reinforcement. This paper outlines the various methods for fabricating SiC nanostructures.

1.  Crystal structure

because of its high Young’s modulus and hardness, excellent

Silicon carbide (SiC) is a promising ceramic for various

oxidation and corrosion durability, high strength at elevatedindustrial applications thanks to its excellent properties.

temperatures, and good thermal shock resistance [3-5].

SiC is a binary compound semiconductor consisting ofMoreover, SiC is a promising semiconducting material for

carbon and silicon, where each atom is sp3-hybridized andapplication in areas of high temperature, high power, highforms four bonds to four other atoms of the opposite kindfrequency and harsh environments. Therefore, the synthesis(Fig. 1). On the other hand, the crystal structure gives riseof SiC for application in electronic devices has been widely

to polytypism, which is a one-dimensional polymorphism.

investigated in recent decades. As a result of its large band

Unlike most other semiconductors, which only occur ingap (2.39, 3.02, 3.26, and 3.33 eV for 3C-SiC, 6H-SiC,

one or two different crystal structures each, SiC exists in

4H-SiC, and 2H-SiC, respectively, at room temperature), SiC

over 250 known polytypes

shows a very high breakdown field (2.12, 2.2, and 2.5 MV/cm[1, 2]. The difference among thefor 3C-SiC, 4H-SiC, and 6H-SiC, respectively) [6].

polytypes is the stacking sequence along the с-axis of thelattice. The cubic polytype is referred to as β-SiC, whereas

In addition, the prominent thermal conductivity of SiC

the hexagonal and rhombohedral structures are referred to as(3.2, 3.7, and 4.9 W/cmK for 3C-SiC, 4H-SiC, and 6H-SiC,

α-SiC. Due to the low stacking-fault energy, it is easy to form

respectively) is typically 2–3 times higher than that ofdifferent SiC polytypes, making it possible to obtain SiC

silicon (1.5 W/cmK), which allows SiC to remove heat more

crystals with different properties for various applications.

efficiently [7].
3.  Synthesis of SiC
3.1

The Acheson process

Many studies have reported on the synthesis of SiC since
the fabrication process initiated by Acheson in 1892. The
overall formation reaction of SiC by the Acheson method canbe described [8] as follows:
SiO2(s) + 3C(s) = SiC(s) + 2CO(g)(1)

Fig.1 Unit cell structure of SiC single crystal [1].
Quartz sand and petroleum coke are generally used as
2.  Properties and applications

the silicon and carbon sources, respectively. This process

SiC has been widely studied for various applications

involves a carbothermal reduction reaction that takes－5－Silicon Carbide and Its Nanostructures

several hours and is usually carried out in an electrical

Microwave heating is another technique that produces fineresistance furnace at temperatures above 2000°C. Due toand uniform SiC powder at lower temperatures and in shorter

the high reaction temperature and long reaction time, thetimes than the conventional processes [24, 25].

synthesized SiC powder has a large particle size and consistsof mostly alpha-phase SiC. Therefore, extensive milling is

3.3 One-dimensional (1D) SiC nanostructuresneeded to convert the as-synthesized product to sinterable

Since the discovery of carbon nanotubes (CNTs) [26] ,powder with a particle size ranging from a few micrometers

a great deal of attention has been paid to the formation

to submicrometers, which is inevitably accompanied byand cha racter ization of other one - di mensional (1D)contamination from the milling media. The drawbacks ofnanostructures, including inorganic materials (metals,

this industrial production process lie in the high energy

ceramics, glass) and organic materials (biomolecules,

consumption and low product purity.

polymers) [27] . Such 1D nanostructures are expected to
improve our understanding of the fundamental concepts of

3.2 SiC nanopowder

the roles of both dimensionality and size on physical and

The physical and chemical properties of a material criticallychemical properties, as well as for potential applications

depend on the grain size of SiC because, for different grainin electronics, optics and materials science. Among thesizes, a significantly different fraction of atoms forms thevarious 1D nanostructures, 1D SiC nanostructures havesurface of the grain. Fine SiC nanopowder is beneficial forbeen extensively studied in recent years and are proventhe sintering process as coarse powder is usually difficult toto have unique electronic [28], field-emitting [29], optical [30],sinter. SiC nanoparticles are also important as a functional

superhydrophobic [31], and mechanical properties [32], which

filler to improve the properties of materials such as polymers

can be ascribed to their low dimensionality, quantum[9, 10], ceramics[11]

and metals[12]

confinement, and shape effects [33-35].

.

SiC nanoparticles can be synthesized by chemical vapor

Various techniques for fabricating 1D SiC nanostructures,deposition (CVD), sol-gel processes, laser gas-phase pyrolysis

particularly SiC nanowires (NWs), have been developedor laser evaporation processes. For example, Hollabaugh et

and can be classified as follows according to the formation

al. synthesized pure SiC nanopowder by CVD using SiCl4

mechanism.

and C2H4 as precursors[13]. Zhu et al. synthesized SiC powder

with an average particle size of 22 nm by conventional CVD

3.3.1 Carbon nanotube/fiber confined reaction. Viera et al. used a plasma technique to prepare SiC

Dai et al. [36] succeeded in synthesizing SiC nanorods having

nanopowder from CH4 and SiH4 gas mixtures [15]. Li et al. [16]similar diameters to those of CNTs (2–30 nm). The spatial

developed a two-step sol-gel process to synthesize SiC fromorientation of the SiC nanorods was randomly distributed inphenol resin/SiO2 hybrid gels. Jin et al.

synthesized fine-agreement with that of the initial CNTs. Pan et al. [29] used

sized β-SiC powder with a particle diameter of ~400 nm by

the same growth approach but spatially oriented CNTs as

combustion synthesis with the aid of a mechanical activation

the starting material, and synthesized arrays of oriented SiC

process.

NWs.

[14]

[17]

The carbothermal reduction reaction has proven to be an

Carbon fibers have also been used as a template for

economical and effective method for synthesizing nanosizedfabricating SiC NWs [37]. The synthesized SiC NWs produced

SiC powder, using various carbon and silicon sources. Martinin this process have uniform cross sections, well-ordered

et al. synthesized nanocrystalline SiC powder from a solution

structures, and very low concentrations of stacking faults.

of sugar in silica sol. Zhang et al. fabricated nanosized SiC

The carbon nanotube/fiber confined reactions containpowder by carbothermal reduction of SiO2 and SiO2-Al 2O3

no catalyst in comparison with 1D SiC nanostructures

xerogels [19]. Yoshioka et al. used a liquid carbon source ofsynthesized by the vapor–liquid–solid (VLS) mechanism.

[18]

phenolic resin and various silica sources to synthesize SiC
powders. Ultra-fine SiC powder with a grain size of 10–30

3.3.2 1D SiC nanostructure growth via the VLS

nm was obtained from TEOS and liquid C by carbothermal

mechanism

reaction at 1600°C [20].

The VLS growth process is the most well-establishedIn addition, extensive research has been done to develop

method for producing 1D SiC nanostructures. The VLS

a method for reducing the temperature of the carbothermal

mechanism introduces a catalytic liquid alloy phase that can

reduction process. For example, high-energy reaction milling

rapidly adsorb a vapor to supersaturation levels and crystal

can synthesize nanosized SiC powder without heating

growth can subsequently occur. The use of a catalyst allows[21–23].
－6－

Jin Li, Takashi Shirai, Masayoshi Fuji

the formation of the liquid phase at low temperatures and fast

one crystallographic direction. An appropriate and well-

growth, contrary to the very slow growth of a crystal throughcontrolled growth configuration must be employed in orderdirect adsorption of a gas phase onto a solid surface. The

to form nanosized nuclei for subsequent growth on top of

1D SiC nanostructures grown by VLS usually have catalyst

them as well as to ensure growth along one axis. The mostparticles on their tips.

important feature is that the reaction develops without thepresence of a metallic catalyst, which could be an advantage
over other methods using a metal catalyst since the presenceof the catalyst in the final product is considered deleterious
for device application.

Fig.4 Schematic illustration of the SiC nanowires growth via
VS mechanism [40].
Fig.2 Schematic illustration of the growth process of theYang et al. fabricated SiC nanowires by a simple catalyst-

aligned 1D nanostructures via VLS mechanism

free method using detonation soot powder and silicon wafers

[38]

.

(Fig. 4) [40]. The nanowires have a diameter of 30–100 nm
Xi et al. developed a novel magnesium-catalyzed co-and a length of 0.5–1.5 μm. The axial growth direction of

reduction route for the large-scale synthesis of aligned β-SiC

each nanowire is preferentially along the κ direction, while

1D nanostructures at a relatively lower temperature of 600°C

a low density of planar defects is detected. A relatively low(Fig.2)threshold field of 6.2 V μm-1 suggests that it is a promising[38]. By carefully controlling the reagent concentration,

β-SiC rod-like and needle-like nanostr uctures can bematerial for flat panel displays.

achieved (Fig. 3) and the as-synthesized β-SiC nanostructures
exhibit strong shape-dependent field emission properties.

3.4 Synthesis of SiC from plant-based biomass

Li et al. synthesized large areas of centimeters-long SiC

Plant-based biomass including rice husk (RH) [41-43], coconut

nanowires through pyrolysis of a polymer precursor withshell [44] , cotton fiber [45] , sugarcane leaf with rice straw

ferrocene as the catalyst by a CVD route [39]. The NWs, with a[46]

length of several centimeters and a diameter of 100–200 nm,

materials for the fabrication of SiC nanostructures. These

were composed of single-crystal β-SiC along the <111>. The

agricultural byproducts contain large amounts of SiO2 and

SiC NWs showed good intense-current emitting properties

C that naturally accumulate at the skin or outer layer andwhen a pulsed high-voltage electric field was imposed.

have a high surface area and close contact. It is possible toand bean-curd refuse [47] have proven to be good raw

form SiC at a relatively low temperature that is far lower thanthat indicated by thermodynamic and kinetic calculations.
Additionally, plant-based biomass is inexpensive andabundantly available all over the world. Among the different
types of biomass, RH has been the most widely studied
Fig.3 Representative SEM images of the as-synthesizedsince the pioneering work by Lee and Cutler in 1975 [41]. The

β-SiC samples: (a) rod-like sample I, (b) rod-like sample II,

extensive studies performed on RH might be due to the highand (c) needle-like sample.

silica content compared to other agricultural byproducts.
The SiC synthesized by RH pyrolysis usually consists of a

3.3.3

1D SiC nanostructure growth via the

mixture of SiC particles and whiskers, with β-SiC as the main

vapor–solid (VS) mechanism

product. The effects of synthesis parameters such as pyrolysis

The VS mechanism cor responds to the case where

temperature, holding time, heating rate and chambersilicon and carbon gaseous precursors react on a solid

atmosphere, etc. have been widely investigated. Our groupsurface to form 1D SiC nanostructures. Growth starts at

synthesized nanostructured β-SiC including particles and 1D

nanometer-sized nuclei created in situ and proceeds along

nanostructures by direct pyrolysis of RH in argon atmosphere－7－

Silicon Carbide and Its Nanostructuresat different temperatures and durations [48, 49]. The results

Microwave heating was carried out in a 2.45 GHz microwave

revealed that a complete carbothermal reduction reaction was

furnace and the complete carbothermal reduction reaction

achieved at 1500°C for 4 h or at 1600°C for 2 h. The β-SiC

could be achieved at 1300°C for 60 min or at 1500°C for

obtained on the bodies of pyrolyzed RH was mainly particles,

only 15 min. As shown in Fig. 7, the products are a mixture

as well as a small amount of β-SiC whiskers. We found thatof SiC particles and whiskers. The SiC particles are 60–130

the pyrolysis temperature and duration greatly influenced

nm in diameter and the whiskers, which are several to tens

the morphology and microstructure of the synthesized SiC.

of micrometers in length, have a diameter of 110–170 nm.

As shown in Fig. 5, the β-SiC particles obtained at 1600°C

Compared to the conventional heating method, microwave

for 2 h had the smallest particle size of 100–200 nm. On theheating proved to be an efficient approach for the synthesis

other hand, 1D β-SiC nanostructures were obtained from theof SiC in terms of energy and time saving, as well as for thevapor-deposited products formed on the graphite crucible

fabrication of nanostructured SiC.

walls (Fig. 6). The β-SiC/SiO2 nanochains were synthesized
at 1500°C for 2 h. Pure β-SiC whiskers with a diameter of~160 nm and tens of micrometers in length were obtained
at 1500°C for 4 h. As the pyrolysis temperature increased,
β-SiC whiskers showed a shorter length, larger diameter andlower density of stacking faults.

Fig. 7 Low magnification FE-SEM images of the β-SiC
Fig. 5 FE-SEM images of β-SiC particles obtained at

powders synthesized at (a) 1300 ºC for 60 min and (b)different temperature and duration.

1500 ºC for 15 min by microwave heating method; highmagnification FE-SEM images of (c and d) β-SiC whiskers
and (e and f) β-SiC particles.
4.  Conclusions
Various SiC nanostructures, especially 1D SiC nanowires,
have been grown by a variety of methods via different growthFig. 6 FE-SEM images of the 1D nanostructures obtained onmechanisms. Each method shows specific advantages and it

the inner walls of graphite crucible by direct pyrolysis of RH

is difficult to conclude which method and growth mechanism

in argon atmosphere at different temperatures and durations:

results in the best quality of nanostructured SiC suitable(a,b) 1500°C-2h; (c,d) 1500°C-4h; (e, f) 1500°C-6h; (g, h)

for all applications. The cost of precursors, the operation

1600°C-2h; (i , j) 1700°C-2h.

temperature, the yield and morphology of the products, andthe feasibility of synthesis procedures on a large scale should
be considered as a whole.

Our group developed a two-step method for fabricating
nanostructured SiC from RH by microwave heating [50] .

The synthesis of SiC and its nanostructures from plant-basedFirst, the raw RH was carbonized in Ar at 700–1000°C bybiomass, especially rice husk, is an economical and simple

a vertical graphite furnace to obtain carbonized rice husk

approach due to its high activity and low cost. However,(CRH) and then was ball-milled to form CRH powder,

several matters still need to be addressed to improve thiswhich showed excellent microwave absorbance performance.

method, such as the purity of the product formed, the ability－8－

Jin Li, Takashi Shirai, Masayoshi Fuji

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