催化剂、温度和保护气体对微硅粉合成碳化硅晶须的影响
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摘要
以工业废弃物微硅粉为硅源,石墨为碳源,硼酸为催化剂,采用碳热还原法制备碳化硅晶须。通过XRD及SEM对合成产物的物相及形貌进行分析,探讨了碳源、合成温度、催化剂加入量和保护气体对合成碳化硅晶须的影响。结果表明:选择石墨为碳源可成功制备出碳化硅晶须;合成温度为1550℃和1650℃时,所制备的晶须呈直线状,表面平直光滑,而当温度为1600℃时,晶须呈竹节状;以氮气为保护气体,催化剂的含量为5%～6%时,合成的晶须的产率最高,且品质好,晶须在氮气中的生长机理推测为气固机理。该合成方法为工业废弃物微硅粉的高质化利用提供了一条切实可行的路线。
The present work describes an economical and simple synthesis strategy for the fabrication of Si C whiskers using industrial waste product. Carbothermal reduction route is used for the reduction of silicon dioxide from the silica fume in the presence of suitable catalyst. It has been observed that the growth rate and product morphology are significantly affected by the process temperature,catalyst and inert gas. It is found that Si C whiskers can be successfully synthesized by using graphite as carbon source. The as-synthesized Si C whiskers are smooth,straight and long at 1550 ℃ or 1650 ℃. However,they have bamboo-like morphology at temperature of 1600 ℃. The products quality is good and the yield is high when the content of catalyst is 5%-6% and N2 is used as protective gas. The tentative growth mechanism is vapor-solid mechanism. This synthesis strategy is resourceful in utilizing the industrial waste product silica fume.
The present work describes an economical and simple synthesis strategy for the fabrication of Si C whiskers using industrial waste product. Carbothermal reduction route is used for the reduction of silicon dioxide from the silica fume in the presence of suitable catalyst. It has been observed that the growth rate and product morphology are significantly affected by the process temperature,catalyst and inert gas. It is found that Si C whiskers can be successfully synthesized by using graphite as carbon source. The as-synthesized Si C whiskers are smooth,straight and long at 1550 ℃ or 1650 ℃. However,they have bamboo-like morphology at temperature of 1600 ℃. The products quality is good and the yield is high when the content of catalyst is 5%-6% and N2 is used as protective gas. The tentative growth mechanism is vapor-solid mechanism. This synthesis strategy is resourceful in utilizing the industrial waste product silica fume.
引文
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[3]张金梁,郭占成,支歆,等.微硅粉中SiO2在稀碱液中的溶解行为及动力学[J].过程工程学报,2012,12(2):212-217.
[4]宋祖伟,李旭云,蒋海燕,等.碳化硅晶须合成工艺的研究[J].无机盐工业,2006,38(1):29-31.
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[8] Raman V,Parashar V K,Bahl O P. Influence of boric acid on the synthesis of silicon carbide whiskers from rice husks and polyacrilonitrile[J].Journal of Materials Science Letters,1997,16(15):1252-1254.
[9] Cheng T W,Hsu C W. A study of silicon carbide synthesis from waste serpentine[J]. Chemosphere,2006,64(3):510-514.
[10] Chol H J,Lee J G. Continuous synthesis of silicon carbide whiskers[J]. Journal of Materials Science,1995,30(8):1982-1986.
[11] Ray K J,Mahanty G. Effect of catalysts and temperature on silicon carbide whiskers formation from rice hustle[J]. Journal of Materials Science Letters,1991,10(7):227-229.
[12]韩敏芳,李伯涛,郭梦熊.碳化硅晶须品质及影响因素[J].人工晶体学报,1996,25(4):343-347.
[13] Belmonte T,Bonnetain L,Ginoux J L. Gas flow nature influence on silicon carbide whiskers synthesis in fixed bed[J]. Vacuum,1996,47(3):291-295.
[14] Wagner R S,Ellis W C. Vapor-Liquid-Solid Mechanism of Single Crystal Growth[J]. Appl. Phys. Lett.,1964,4(5):89-90.
[15]宋祖伟,戴长虹,翁长根.碳化硅晶须的生长机理与制备方法[J].青岛化工学院学报,2001,22(3):242-246.
[2]翟凤瑞.硅粉的形成及应用前景[J].中国资源综合利用,2003,(8):31-34.
[3]张金梁,郭占成,支歆,等.微硅粉中SiO2在稀碱液中的溶解行为及动力学[J].过程工程学报,2012,12(2):212-217.
[4]宋祖伟,李旭云,蒋海燕,等.碳化硅晶须合成工艺的研究[J].无机盐工业,2006,38(1):29-31.
[5]汪耀祖,郭梦熊.稻壳SiC晶须的生长工艺及机理[J].硅酸盐学报,1993,21(1):22-28.
[6] SelvamA,Nair N G. Synthesis and characterization of SiC whiskers from coconut shells[J]. J. Mater. Sci. Let.,1998,17:57-60.
[7] Comer J J. A study of contrast bands inβ-SiC whiskers[J]. Materials Research Bulletin,1969,4(5):279-287.
[8] Raman V,Parashar V K,Bahl O P. Influence of boric acid on the synthesis of silicon carbide whiskers from rice husks and polyacrilonitrile[J].Journal of Materials Science Letters,1997,16(15):1252-1254.
[9] Cheng T W,Hsu C W. A study of silicon carbide synthesis from waste serpentine[J]. Chemosphere,2006,64(3):510-514.
[10] Chol H J,Lee J G. Continuous synthesis of silicon carbide whiskers[J]. Journal of Materials Science,1995,30(8):1982-1986.
[11] Ray K J,Mahanty G. Effect of catalysts and temperature on silicon carbide whiskers formation from rice hustle[J]. Journal of Materials Science Letters,1991,10(7):227-229.
[12]韩敏芳,李伯涛,郭梦熊.碳化硅晶须品质及影响因素[J].人工晶体学报,1996,25(4):343-347.
[13] Belmonte T,Bonnetain L,Ginoux J L. Gas flow nature influence on silicon carbide whiskers synthesis in fixed bed[J]. Vacuum,1996,47(3):291-295.
[14] Wagner R S,Ellis W C. Vapor-Liquid-Solid Mechanism of Single Crystal Growth[J]. Appl. Phys. Lett.,1964,4(5):89-90.
[15]宋祖伟,戴长虹,翁长根.碳化硅晶须的生长机理与制备方法[J].青岛化工学院学报,2001,22(3):242-246.