微波烧结制备碳化硅晶须的影响因素
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摘要
将干燥后的硅溶胶-活性炭作为反应物,在不加入任何金属催化剂的情况下,利用微波加热碳热还原法合成碳化硅晶须,研究反应温度和时间及坩埚部位对产物的影响。结果表明:30 min时,温度由1300℃升高到1600℃,产物中物相β-SiC越来越多;1500℃条件下,合成产物在坩埚的上部和中部主要分别为分散的SiC晶须和团聚在一起的SiC晶须;坩埚底部的产物主要为表面光滑的SiO2颗粒。1600℃条件下,合成产物在坩埚的上部和中部主要分别为分散的SiC晶须和等轴状β-SiC颗粒,底部为晶须和颗粒的混合物。1500℃×30 min得到的SiC晶须产率和直晶率优于1600℃×30 min得到的SiC晶须产率和直晶率。
Silicon carbide whiskers were synthesized by microwave heating carbothermic method using dried silica sol and active carbon as reactants under the condition of no adding any metal catalysts.The effects of heating temperature and time on products were studied.The results show that as the sintering temperature rises from 1300 ℃ to 1600 ℃ under the heating time of 30 min,the amount of β-SiC phase in the product increases.Different products are observed at different positions of the crucible.The products of dispersal SiC whisker and agglomerated SiC whisker at the top part and the center part of the crucible,and smooth surface SiO2 particles at the bottom of the crucible are obtained at the sintering temperature of 1500 ℃ for 30 min.Under the condition of heating temperature at 1600 ℃,the synthetic products are mainly composed of dispersal SiC whisker and equiaxial β-SiC particles at the top part and the center part of the crucible,and a mixture of whiskers and particles at the bottom of the crucible.It is found that higher yield and straight whiskers ratio can be obtained for synthesizing silicon carbon whiskers by microwave sintering at 1500 ℃ for 30 min.
Silicon carbide whiskers were synthesized by microwave heating carbothermic method using dried silica sol and active carbon as reactants under the condition of no adding any metal catalysts.The effects of heating temperature and time on products were studied.The results show that as the sintering temperature rises from 1300 ℃ to 1600 ℃ under the heating time of 30 min,the amount of β-SiC phase in the product increases.Different products are observed at different positions of the crucible.The products of dispersal SiC whisker and agglomerated SiC whisker at the top part and the center part of the crucible,and smooth surface SiO2 particles at the bottom of the crucible are obtained at the sintering temperature of 1500 ℃ for 30 min.Under the condition of heating temperature at 1600 ℃,the synthetic products are mainly composed of dispersal SiC whisker and equiaxial β-SiC particles at the top part and the center part of the crucible,and a mixture of whiskers and particles at the bottom of the crucible.It is found that higher yield and straight whiskers ratio can be obtained for synthesizing silicon carbon whiskers by microwave sintering at 1500 ℃ for 30 min.
引文
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[2]李缨,黄凤萍,梁振海.碳化硅陶瓷的性能与应用[J].陶瓷,2007,33(5):36-37.LI Ying,HUANG Feng-ping,LIANG Zhen-hai.Properties and applications of silicon carbide ceramic[J].Ceramics,2007,33(5):36-37.
[3]Katharria Y S,Kumar S,Ram P,et al.Characterizations of pulsed laser deposited SiC thin films[J].Journal of Non-Crystalline Solids,2007,353(52):4660-4665.
[4]Suzuki H,Araki H,Tosa M,et al.SiC film formation from fluorosilane gas by plasma CVD[J].Journal of Crystal Growth,2006,294(2):464-468.
[5]宁叔帆,刘晓霞,马勇,等.SiC晶须制备方法及应用[J].西安石油大学学报:自然科学版,2004,19(1):66-69.NING Shu-fan,LIU Xiao-xia,MA Yong,et al.Preparation and applications of silicon carbide whiskers[J].Journal of Xi’an Shiyou University:NaturalScience Edition,2004,19(1):66-69.
[6]罗军明,魏峥,艾云龙,等.微波烧结温度对WC钢结硬质合金组织性能的影响[J].材料热处理学报,2011,32(7):31-36.LUO Jun-ming,WEI Zheng,AI Yun-long,et al.Effect of microwave sintering temperature on microstructure and properties of WC steel-bondedcemented carbide[J].Transactions of Materials and Heat Treatment,2011,32(7):31-36.
[7]Satapathy L N,Ramesh P D,Dinesh A,et al.Microwave synthesis of phase-pure,fine silicon carbide powder[J].Materials Research Bulletin,2005,40(10):1871-1882.
[8]张涛,王德仁,何业东.微波热处理制备硅化物涂层及其抗高温氧化性能[J].材料热处理学报,2011,32(12):125-131.ZHANG Tao,WANG De-ren,HE Ye-dong.Preparation and high-temperature oxidation resistance of silicide coating by microwave heat treatment[J].Transactions of Materials and Heat Treatment,2011,32(12):125-131.
[9]万隆,李德意,刘文超,等.温度对碳热还原合成SiC晶须的影响[J].陶瓷学报,2001,22(4):222-223.WAN Long,LI De-yi,LIU Wen-chao,et al.Influence of temperature on the synthetic whisker SiC by carbon thermal reducion method[J].Journal ofCeramics,2001,22(4):222-223.
[10]Lee J C,Cutter I B.Formation of silicon carbide from rice hulls[J].American Ceramic Society Bulletin,1975,54(2):195-197.
[11]张克从,张乐江.晶体生长[M].北京:科学出版社,1981.
[12]Kevorkijan,Komac V,Kolar M.Low-temperature synthesis of sinterable SiC powders by carbothermic reduction of colloidal SiO2[J].Journal ofMaterial Science,1992,27(10):5-12.