非水解溶胶—凝胶碳热还原氮化法制备TiN粉体研究  

Synthesis of TiN Powders Via Carbothermal Reduction Nitridation Process Based on Non-hydrolytic Sol-gel Method

作　　者：崔燚[1,2,3] 卜景龙[1,3] 魏恒勇[1,2,3] 王瑞生[1,3] 魏颖娜[1,3] 于云[2] 于洋[2] 严昊苏 

机构地区：[1]河北联合大学材料科学与工程学院,河北唐山063009 [2]中国科学院特种无机涂层重点实验室,上海200050 [3]河北省无机非金属材料重点实验室,河北唐山063009 [4]上海应用技术学院工程创新学院,上海201418

出　　处：《陶瓷》2014年第1期26-30,共5页Ceramics

基　　金：国家自然科学基金(项目编号:51272066);河北省自然科学基金(项目编号:E2013209183);中国科学院特种无机涂层重点实验室开放课题基金(项目编号:KLICM-2011-01);河北省高等学校科学技术研究青年基金项目(项目编号:2011124)

摘　　要：首先,以四氯化钛为原料,异丙醚为氧供体,二氯甲烷为溶剂,采用非水解溶胶-凝胶法合成高活性的TiO2凝胶;其次以其为钛源,选用分子量为1 300 000的聚乙烯吡咯烷酮为碳源,采用碳热还原氮化法合成TiN粉体。X射线衍射仪、场发射扫描电镜和激光粒度仪测试结果表明,与水解法相比,采用非水解法合成的TiO2凝胶经800℃煅烧0.5h仍为活性较高的锐钛矿相,以该凝胶为钛源,经1 200℃碳热还原氮化2h可合成纯度相对较高的TiN粉体,将合成温度升至1 300℃还原氮化5h可合成更高纯度的TiN粉体。TiN粉体颗粒呈近似球形,发育较好,粒径在1μm以下,激光粒度测定粒径主要集中在10μm左右,d50为8μm。Titanium dioxide gel precursor was prepared by non--hydrolytic sol--gel method with titanium tetrachloride as raw materials, isopropyl ether as oxygen donor and dichloromethane as solvent, respectively. The TiN powders were syn- thetized by carbothermal reduction nitridation method with the non--hydrolytic TiO2 gel precursor as titanium source and polyvinylpyrrolidone （molecular weight 1300000） as carbon source, respectively. The TiN powders were investigated by XRD, FE--SEM and laser particle analysis. The results show that there was only anatase phase when the non--hydrolytic TiO2 gel was calcined at 800℃ for 0.5 h. Using the non--hydrolytic TiO2 gel as titanium source, the TiN powders could be synthetized at 1 200 ℃ for 2 h by carbothermal reduction nitridation process. TiN powders with higher purity would be syn thetized when carbothermal reduction nitridation temperature was at 1 300 ℃ for 5 h. The TiN powders were nearglobular particle and their particle size was less than 1 fire. The laser particle size analysis result show that the TiN powders were mainly distributed in about 10 μm, and the d50 value was 8 fire.

关 键 词：非水解溶胶-凝胶法 碳热还原氮化法 氮化钛 粉体 

分 类 号：TQ174.4[化学工程—陶瓷工业]