Low Temperature Catalytic Synthesis of β-SiC Powders via Microwave Heating

doi:10.15541/jim20160541

Abstract

Abstract:

β-SiC powders were synthesized by a microwave heating method at 1150℃ for 30 min under Ar atomosphere using silicon powders and phenolic resin as raw materials, and nickel nitrate as catalyst precursor. The effects of temperature, catalyst content and holding time on the formation of SiC were investigated. XRD, SEM and TEM were used to characterize the phase and microstructure of the prepared samples. It indicated that β-SiC can be synthesized at 1150℃ for 0.5 h by using 1.0wt% Ni as catalysts. In contrast, for the sample prepared without Ni catalysts, corresponding preparation temperature of β-SiC was as high as 1250℃. Both β-SiC whiskers and particles were formed in the samples prepared with or without catalysts, and the length of formed β-SiC whiskers in the samples prepared with Ni catalysts were larger than those without catalyst. Density functional theory (DFT) calculation shows that the formation of Ni-Si alloy can elongate the length of Si-Si chemical bond, weaken its bond strength, and finally accelerate the carbonization reaction of Si powder at a relative low temperature.

Key words: β-SiC, microwave heating, catalytic-reaction, density functional theory

CLC Number:

TB35

WANG Jun-Kai, ZHANG Yuan-Zhuo, LI Jun-Yi, ZHANG Hai-Jun, LI Fa-Liang, HAN Lei, SONG Shu-Peng. Low Temperature Catalytic Synthesis of β-SiC Powders via Microwave Heating[J]. Journal of Inorganic Materials, 2017, 32(7): 725-730.

Figures/Tables 8

Fig. 1 XRD patterns of samples reacted at various temperatures for 0.5 h without any catalysts(Si: JCPDS 01-077-2109; SiC: JCPDS 01-073-1708)

Fig. 2 XRD patterns of samples reacted at various temperatures for 0.5 h with 2 wt% Ni catalysts(Si: JCPDS 01-077-2109; SiC: JCPDS 01-073-1708)

Fig. 3 XRD patterns of samples reacted at 1150℃ for 0.5 h with various contents of Ni catalysts(Si: JCPDS 01-077-2109; SiC: JCPDS 01-073-1708)

Fig. 4 XRD patterns of samples reacted at 1150℃ for various holding time with 1.0wt% Ni catalysts(Si: JCPDS 01-077-2109; SiC: JCPDS 01-073-1708)

Fig. 5 SEM images of the as-prepared β-SiC(a) 1250℃/0.5 h, without catalyst; (b) 1150℃/0.5 h, with 1.0wt% Ni as catalyst

Fig. 6 TEM ((a) low-and (b) high-magnification), SAED (c) and HR-TEM (d) images of as-prepared β-SiC whiskers

Table1 Total energies and cohesive energies of Si55, Si43Ni12 and Si37Ni18 clusters

Clusters composition	Single Si atom	Single Ni atom	Si₅₅	Si₄₃Ni₁₂	Si₃₇Ni₁₈
Total energy/(a.u.)	-290.133	-1390.136	-15957.557	-30668.916	-38024.613
Cohesive energy/(kJ·mol^-1)	—	—	582.458	940.142	1165.307

Fig. 7 The DFT calculations of bond length of Si atoms at edge sites0 on (111) face of Si55 (a), Si43Ni12 (b) and Si37Ni18 (c) clusters

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