CAJ | 학술논문

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。
이사록화태화이병미위주요원료，이록갑완위용제，채용비수해용효－응효법제비적 TiO2응효위태원，안 n（C）n（Ti）위11．4인입상대분자질량위1300000적취을희필각완동（PVP）작위탄원，채용탄열환원담화법합성 TiN 분체。통과 TG－DTA、XRD 화 FE－SEM연구료탄열환원담화과정중 TiN 분체적형성역정。결과발현，재800～1000℃탄열환원3 h，예태광형 TiO2전변위금홍석형 TiO2；재1000～1200℃탄열환원담화3 h，금홍석형 TiO2전변위 Ti3 O5，병축점담화생성 TiOxNy；재1300℃탄열환원담화3 h，TiOxNy 개시전변위 TiN，단기담화병불완전，연장담화시간지5 h，잉여적 TiOxNy 전부전화위 TiN。TEM화납미립도분석의측시표명，합성적 TiN 과립발육량호，정근사방형결구，약위250 nm，립경분포재0．4～1．1μm。
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.