煤源灰分对煤基SiC纳米结构及堆积缺陷的影响
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摘要
以电锻太西煤和未电锻太西煤为原料,采用溶胶凝胶法制备纳米级煤质碳化硅材料,并对其结构进行XRD,TEM,XPS表征及计算分析。研究发现,以高灰分的未脱灰电锻太西煤碳源所制备的SiC材料中,其堆积缺陷变化较大,且随着催化剂用量的增加其微观形貌呈现棒状、线状及颗粒状;而当催化剂用量一定时,以低灰分的脱灰电锻太西煤为原料所获得的SiC材料结构中堆积缺陷密度随其原料灰分的升高而下降,当灰分为4. 43%时,碳化硅堆积缺陷变化不明显,且其微观形貌保持均一。碳源灰分与催化剂在一定范围内,对于调控纳米碳化硅的形貌、比表面积等具有一定协调催化作用,可以通过催化剂及灰分调控以控制获得不同纳米形态的碳化硅材料。
Nano-scale coal-based silicon carbide materials were prepared by electro-forging Taixi coal and non-electric forging Taixi coal,and the structure was characterized by XRD,TEM,XPS and calculation.The results show that the SiC materials prepared by high-ash unashed electric forging Taixi coal carbon source have large variation of stacking defects,and their morphology is rod-shaped,linear and granular with increasing catalyst dosage. When the amount of catalyst is constant,the bulk defect density of SiC material structure obtained by low-ash de-ashing electric forging Taixi coal as raw material decreases with the increase of raw material ash; when ash is 4. 43%,silicon carbide accumulation defect the change is not obvious and its microscopic morphology remains uniform. The ash and catalyst of the carbon source have a certain coordination effect on the morphology and specific surface area of the nano-SiC,and the silicon carbide materials with different nano-morphologies can be controlled by catalyst and ash.
Nano-scale coal-based silicon carbide materials were prepared by electro-forging Taixi coal and non-electric forging Taixi coal,and the structure was characterized by XRD,TEM,XPS and calculation.The results show that the SiC materials prepared by high-ash unashed electric forging Taixi coal carbon source have large variation of stacking defects,and their morphology is rod-shaped,linear and granular with increasing catalyst dosage. When the amount of catalyst is constant,the bulk defect density of SiC material structure obtained by low-ash de-ashing electric forging Taixi coal as raw material decreases with the increase of raw material ash; when ash is 4. 43%,silicon carbide accumulation defect the change is not obvious and its microscopic morphology remains uniform. The ash and catalyst of the carbon source have a certain coordination effect on the morphology and specific surface area of the nano-SiC,and the silicon carbide materials with different nano-morphologies can be controlled by catalyst and ash.
引文
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[4]Gianchandani P K,Casalegno V,Salvo M,et al.SiC foam sandwich structures obtained by Mo-wrap joining[J].Materials Letters,2018,221:240-243.
[5]吴旭峰,凌一鸣.电弧放电制备碳化硅纳米棒[J].硅酸盐学报,2006,34(10):1283-1286.
[6]Shi Y F,Meng Y,Chen D H,et al.Highly ordered mesoporous silicon carbide ceramics with large surface areas and high stability[J].Advanced Functional Materials,2006,16(4):561-567.
[7]Wu R,Zhou K,Yang Z,et al.Molten-salt-mediated synthesis of Si C nanowires for microwave absorption application[J].Cryst.Eng.Comm.,2013,15(3):570-576.
[8]Xiao J,Li F,Zhong Q,et al.Separation of aluminum and silica from coal gangue by elevated temperature acid leaching for the preparation of alumina and SiC[J].Hydrometallurgy,2015,155:118-124.
[9]Safi S,Rad R Y.In situ synthesis of nano size silicon carbide and fabrication of C-SiC composites during the siliconization process of mesocarbon microbeads preforms[J].Ceramics International,2012,38(6):5081-5087.
[10]Seo W S,Koumoto K.Stacking faults inβ-SiC formed during carbothermal reduction of SiO2[J].Journal of the American Ceramic Society,1996,79(7):1777-1782.
[11]Nyathi M S,Burgess Clifford C,Schobert H H.Effect of petroleum feedstock and reaction conditions on the structure of Coal-petroleum Co-cokes and Heat-treated products[J].Energy Fuel,2012,26(7):4413-4419.
[12]Ahmed Y M Z,El-Sheikh S M.Influence of the pH on the morphology of sol-gel derived nanostructured SiC[J].Journal of the American Ceramic Society,2009,92(11):2724-2730.
[13]Zhang Y F,Tang Y H,Wang N,et al.Silicon nanowires prepared by laser ablation at high temperature[J].Applied physics letters,1998,72(15):1835-1837.
[14]Duan X,Lieber C M.General synthesis of compound semiconductor nanowires[J].Advanced Materials,2000,12(4):298-302.
[15]Chiu S C,Lin W H,Wu H C,et al.Silicon carbide nanowire as nanoemitter and greenish-blue nanophosphor for field emission applications[J].Nanoscience and Nanotechnology Letters,2012,4(1):72-76.
[16]Milewski J V,Gac F D,Petrovic J J,et al.Growth of beta-silicon carbide whiskers by the VLS process[J].Journal of materials Science,1985,20(4):1160-1166.
[17]Liu Z,Ci L,Jin-Phillipp N Y,et al.Vapor-solid reaction for silicon carbide hollow spherical nanocrystals[J].The Journal of Physical Chemistry C,2007,111(34):12517-12521.
[18]Cao G.Synthesis,Properties and Applications[M].London:Imperial college press,2004.
[19]Frank F C.The influence of dislocations on crystal growth[J].Discussions of the Faraday Society,1949,5:48-54.
[20]Blakely J M,Jackson K A.Growth of crystal whiskers[J].The Journal of Chemical Physics,1962,37(2):428-430.
[21]Seo W S,Koumoto K,Aria S.Morphology and stacking Faults ofβ-silicon carbide whisker synthesized by arbothermal reduction[J].Journal of the American Ceramic Society,2000,83(10):2584-2592.
[22]Martin H P,Ecke R,Müller E.Synthesis of nanocrystalline silicon carbide powder by carbothermal reduction[J].Journal of the European Ceramic Society,1998,18(12):1737-1742.
[23]Morales A M,Lieber C M.A laser ablation method for the synthesis of crystalline semiconductor nanowires[J].Science,1998,279(5348):208-211.