采用长链甲基三甲氧基硅烷〔Cn H2 n+ 1 Si(OCH3)〕和正硅酸乙酯 (TEOS)两种有机物为起始原料 ,用溶胶 -凝胶法通过合理控制反应条件 ,制备出β- Si C凝胶粉体 ,然后在 Ar气氛、 90 0～ 130 0℃下热处理 ,制备出了高纯、低氧含量 ,直径 2～ 10 nm,长度 40～ 80 nm的β- Si C纳米晶须。产物纯度达到 99.92 %。利用 X射线粉晶衍射、透射电镜 (TEM)、拉曼光谱等测试方法对制得的晶须进行了结构及颗粒尺寸等研究。讨论了反应条件对β- Si C纳米晶须生长的影响 The long-chain methyltrimethoxysilane [Cn H2 n + 1 Si (OCH3)] and tetraethyl orthosilicate (TEOS) were used as starting materials. By controlling the reaction conditions by sol-gel method, - Si C gel powder and then heat treated at 90 0 ~ 130 0 ℃ in Ar atmosphere to prepare β-Si C nanocrystals with high purity and low oxygen content, diameter of 2 ~ 10 nm and length of 40 ~ 80 nm Must The purity of the product reached 99.92%. The structure and particle size of the prepared whiskers were investigated by X-ray powder diffraction, transmission electron microscopy (TEM) and Raman spectroscopy. The effects of reaction conditions on the growth of β-Si C nanowhiskers were discussed