Catalytic Carbothermal Reduction Synthesis and Mechanism of 3C-SiC from Diatomite with Fe as Catalyst

doi:10.11901/1005.3093.2017.533

Chinese Journal of Materials Research

2018, Vol. 32

Issue (10): 767-774 DOI: 10.11901/1005.3093.2017.533

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Catalytic Carbothermal Reduction Synthesis and Mechanism of 3C-SiC from Diatomite with Fe as Catalyst

Junkai WANG, Yuanzhuo ZHANG, Saisai LI, Shengtao GE, Jianbo SONG, Haijun ZHANG(

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The State Key Laboratory of Refractories and Metallurgy, Wuhan University of Science and Technology, Wuhan 430081, China

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Junkai WANG, Yuanzhuo ZHANG, Saisai LI, Shengtao GE, Jianbo SONG, Haijun ZHANG. Catalytic Carbothermal Reduction Synthesis and Mechanism of 3C-SiC from Diatomite with Fe as Catalyst. Chinese Journal of Materials Research, 2018, 32(10): 767-774.

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Abstract

Nanopowders of 3C-SiC were synthesized at 1400°C for 3 h in Ar atmosphere via catalytic carbothermal reduction reaction method with industrial diatomite powders and phenolic resin as raw materials and ferric nitrate as catalyst precursor. XRD, SEM and TEM analysis were employed to characterize the phase composition and microstructure of the final products. The effect of temperature, catalyst content and holding time on the formation of the SiC powders was investigated. The results show that: 1) 3C-SiC can be synthesized at 1400°C for 3 h with 1.0% (mass fraction) Fe as catalyst. In the contrast, for the case without Fe catalyst, only small amount of 3C-SiC was obtained in the final products under identical condition; 2) The as-prepared 3C-SiC nanopowders are granular in morphology, and the diameters of most particles are in nano-scales; 3) Density Functional Theory (DFT) calculation results further show that the Fe catalyst played important role in breaking the Si-O chemical bond.

Key words: inorganic ceramic materials 3C-SiC catalytic carbothermal reduction reaction diatomite density functional theory

Received: 11 September 2017

ZTFLH:

TB332

Fund: Supported by National Natural Science Foundation of China (Nos. 51472184 & 51472185), and Program for Innovative Teams of Outstanding Young and Middle-aged Researchers in the Higher Education Institutions of Hubei Province (No. T201602)

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	Junkai WANG
	Yuanzhuo ZHANG
	Saisai LI
	Shengtao GE
	Jianbo SONG
	Haijun ZHANG

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https://www.cjmr.org/EN/10.11901/1005.3093.2017.533 OR https://www.cjmr.org/EN/Y2018/V32/I10/767

Table 1 Chemical composition of diatomite powders

Fig.1 XRD patterns of samples fired at various temperatures for 3 h without any catalysts (SiO₂: JCPDS No. 01-071-0785; SiC: JCPDS No. 01-073-1708; Graphite: JCPDS No. 01-075-1621)

Fig.2 XRD patterns of samples fired at various temperatures for 3 h with 2.0% Fe catalysts (SiO₂: JCPDS No. 01-071-0785; SiC: JCPDS No. 01-073-1708; Graphite: JCPDS No. 01-075-1621)

Fig.3 Contents of crystalline phases of samples fired at various temperatures for 3 h with 2.0% Fe catalysts

Fig.4 XRD patterns of samples fired at 1400℃ for various holding time with 2.0% Fe catalysts (SiO₂: JCPDS No. 01-071-0785; SiC: JCPDS No. 01-073-1708; C: JCPDS No. 01-075-1621)

Fig.5 Contents of crystalline phases of samples fired at 1400℃ for various holding time with 2.0% Fe catalysts

Fig.6 XRD patterns of samples fired at 1400℃ for 3 h with various contents of Fe catalysts (SiO₂: JCPDS No. 01-071-0785; SiC: JCPDS No. 01-073-1708; C: JCPDS No. 01-075-1621)

Fig.7 Contents of crystalline phases of samples fired at 1400℃ for 3 h with various contents of Fe catalysts

Fig.8 SEM images and corresponding EDS results of the as-prepared SiC powders (a) (b) SEM images (c) EDS results of selected point 1 in Fig. 8a

Fig.9 TEM (a and b), SAED (c) and HRTEM (d) images of as-prepared 3C-SiC powders

Fig.10 SEM image of the as-received diatomite powders

Fig.11 The DFT calculation models (a) Fe₄ clusters, (b) (2×2)SiO₂ (101), and (c) Fe₄-(2×2)SiO₂ (101) (black ball: Fe; red ball: O; yellow ball: Si)

Table 2 Bond lengths of Si-O in the surface of SiO₂ (101): before and after Fe₄ adsorption

Fig.12 Schematic illustrations of the synthesis of SiC nanopowder

[1]	Chiew Y L, Cheong K Y.A review on the synthesis of SiC from plant-based biomasses[J]. Mater Sci Eng B, 2011, 176(13): 951
[2]	Zekentes K, Rogdakis K.SiC nanowires: material and devices[J]. J Phys D: Appl Phys, 2011, 44(13): 133001
[3]	Wu R, Zhou K, Yue C Y, et al.Recent progress in synthesis, properties and potential applications of SiC nanomaterials[J]. Prog Mater Sci, 2015, 72: 1
[4]	Tan C, Liu J, Zhang H, et al.Low temperature synthesis of 2H-SiC powders via molten-salt-mediated magnesiothermic reduction[J]. Ceram Int, 2017, 43(2): 2431
[5]	Shi L, Zhao H, Yan Y, et al.Synthesis and characterization of submicron silicon carbide powders with silicon and phenolic resin[J]. Powder Technol, 2006, 169(2): 71
[6]	Zhao H, Shi L, Li Z, et al.Silicon carbide nanowires synthesized with phenolic resin and silicon powders[J]. Physica E, 2009, 41(4): 753
[7]	Wang J K, Li J Y, Liang F, et al.Low-temperature catalytic synthesis of SiC powders using phenolic resin as carbon resource[J]. J Chin Ceram Soc, 2016, 44(12): 1798(王军凯, 李俊怡, 梁峰等. 以酚醛树脂为碳源低温催化反应合成碳化硅粉体[J]. 硅酸盐学报, 2016, 44(12): 1798)
[8]	Wang J, Zhang Y, Li J, et al.Low temperature catalytic synthesis of β-SiC powders via microwave heating[J]. J Inorg Mater, 2017, 31(7): 725
[9]	Wang J, Zhang Y, Li J, et al.Catalytic effect of cobalt on microwave synthesis of β-SiC powder[J]. Powder Technol, 2017, 317: 209
[10]	Bao Z, Weatherspoon M R, Shian S, et al.Chemical reduction of three-dimensional silica micro-assemblies into microporous silicon replicas[J]. Nature, 2007, 446(7132): 172
[11]	Matovic B, Saponjic A, Devecerski A.Fabrication of SiC by carbothermal-reduction reactions of diatomaceous earth[J]. J Mater Sci, 2007, 42(14): 5448
[12]	?aponji? A, Matovi? B, A. D, et al. Preparation of nanosized non-oxide powders using diatomaceous earth[J]. Sci Sinter, 2009, 41(2): 151
[13]	?aponji? A, Matovi? B, Babi? B, et al.Cost-effective synthesis of Si3N4-SiC nanocomposite powder[J]. Optoelectron Adv Mat, 2010, 4(11): 1681
[14]	Delley B.From molecules to solids with the DMol3 approach[J]. J Chem Phys, 2000, 113(18): 7756
[15]	Perdew J P, Burke K, Ernzerhof M.Generalized gradient approximation made simple[J]. Phys Rev Lett, 1996, 78(18): 3865
[16]	Zhang J, Yan S, Jia Q, et al.Preparation of SiC/SiO2 core-shell nanowires via molten salt mediated carbothermal reduction route[J]. Physica E, 2016, 80: 19
[17]	Xin L, Shi Q, Chen J, et al.Morphological evolution of one-dimensional SiC nanomaterials controlled by sol-gel carbothermal reduction[J]. Mater Charact, 2012, 65: 55
[18]	Wang J K, Zhang H J, Liang F, et al.Effect of pore structure on preparation of carbon nanotubes via pyrolysis of phenolic resin[J]. J Chin Ceram Soc, 2017, 45(3): 416(王军凯, 张海军, 梁峰等. 孔结构对热解酚醛树脂制备碳纳米管的影响[J]. 硅酸盐学报, 2017, 45(3): 416.)
[19]	Wang J, Deng X, Zhang H, et al.Synthesis of carbon nanotubes via Fe-catalyzed pyrolysis of phenolic resin[J]. Physica E, 2017, 86: 24

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