以四氯化钛和异丙醚为主要原料，二氯甲烷为溶剂，采用非水解溶胶－凝胶法制备的 TiO2凝胶为钛源，按 n（C）n（Ti）为11．4引入相对分子质量为1300000的聚乙烯吡咯烷酮（PVP）作为碳源，采用碳热还原氮化法合成 TiN 粉体。通过 TG－DTA、XRD 和 FE－SEM研究了碳热还原氮化过程中 TiN 粉体的形成历程。结果发现，在800～1000℃碳热还原3 h，锐钛矿型 TiO2转变为金红石型 TiO2；在1000～1200℃碳热还原氮化3 h，金红石型 TiO2转变为 Ti3 O5，并逐渐氮化生成 TiOxNy；在1300℃碳热还原氮化3 h，TiOxNy 开始转变为 TiN，但其氮化并不完全，延长氮化时间至5 h，剩余的 TiOxNy 全部转化为 TiN。TEM和纳米粒度分析仪测试表明，合成的 TiN 颗粒发育良好，呈近似方形结构，约为250 nm，粒径分布在0．4～1．1μm。
TiO2 gel was prepared by non-hydrolytic sol -gel method using titanium tetrachloride and isopro-pyl ether as raw materials,and dichloromethane as solvent.TiN powders were synthesized by carbothermal reduction and nitridation of TiO2 gel as titanium source and polyvinyl pyrrolidone (PVP,molecular weight 1300 000)as carbon source based on 11.4 of n(C)n(Ti).The synthesis mechanism of TiN powders was investigated by TG -DTA,XRD and FE -SEM during carbothermal reduction and nitridation.The result shows that anatase TiO2 transforms to rutile TiO2 during carbothermal reduction and nitridation at 800 -1 000℃ for 3 h;rutile TiO2 transforms to Ti 3 O5 ,then to TiOxN y gradually during carbothermal reduction and nitri-dation at 1 000 -1 200 ℃ for 3 h;TiN appears gradually during carbothermal reduction and nitridation at 1 300 ℃ for 3 h,and the nitridation is not complete,but TiOxN y is converted completely to TiN when the nitri-dation time is lengthened to 5 h.The results of TEM micrographs and nano particle size distribution show that TiN crystals of approximate square structure are synthesized well with about 250 nm of dimensions, and the particle size is between 0.4 and 1.1 μm.
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