溶胶-凝胶和碳热还原法制备碳化钛的研究  

Research on synthesis of TiC by sol-gel and carbothermal reduction method

作　　者：黎茂祥[1] 苏国钧[1] 

机构地区：[1]湘潭大学,湖南湘潭411105

出　　处：《无机盐工业》2007年第7期36-38,47,共4页Inorganic Chemicals Industry

摘　　要：以钛酸四丁酯和酚醛树脂为原料，乙二醇甲醚为溶剂，冰乙酸为稳定剂，在硝酸的催化下制备出凝胶前驱体，再将制得的前驱体于流通的氩气环境中经高温碳热还原得到碳化钛。讨论了各因素对凝胶时间的影响，用TG，XRD和SEM对制得的前驱体和产品进行了表征。结果表明，控制溶液的pH在2～3，水与钛酸四丁酯的物质的量比为6：1，溶剂与钛酸四丁酯的体积比为4：1时，得到的凝胶红棕色透明，所需时间最短；且由XRD和SEM分析可知，碳热还原反应是由TiO2经历一系列的低价态氧化物转变完成的；前驱体在氩气环境中经1400℃反应1h后生成的产物为TiC，其表面光洁，粒径分布均匀，大小为0．1～0．5μm。The precursor of gel was prepared firstly by using Ti（ C4 H9O ） 4 and phenolic resin as the raw materials, ethylene glycol monomethyl ether as the solvent, glacial acetic acid as stabilizer and nitric acid as catalyzer. Then the precursor was reduced into TiC by high temperature carbothermal method in flowing argon atmosphere. The influence of various factors on gelation time was discussed. The precursor and product were characterized by TG, XRD and SEM. The results showed that translucent red - brown gel was obtained with the shortest gelation time, when the pH value of the solution was 2 - 3, the amount - of - substance ratio of H2O to Ti （ C4 H9O ） 4 was 6, and the volume ratio of solvent to Ti （ C4 H9O ） 4 was 4： 1. From the analysis of XRD and SEM, the carbothermal reduction reaction was completed by a series lower oxidation of TiO2. It also proved that the product of precursor was TiC when it reacted at the temperature of 1 400 ℃ for 1 h in flowing argon atmosphere. The product has smooth surface and uniform particle size distribution with average size of 0.1 - 0.5 μm.

关 键 词：溶胶-凝胶 碳热还原 酚醛树脂 碳化钛 

分 类 号：TQ134.11[化学工程—无机化工]