将质量比为1:4的TiCl4和NaN。放入不锈钢反应釜内,以二甲苯为溶剂,填充率为60%,用溶剂热方法,在温度340℃,保温24h,制得粉体。粉体分别经二甲苯,无水乙醇、蒸馏水洗涤,105℃干燥和直接经700℃煅烧2h,XRD测试表明:制备出的氮化钛粉体为纳米立方相粉体,晶格常数a=0.4241nm,平均粒径为11.04nm,700℃煅烧后全部转化为TiO2和Ti的混合物;IR测试表明在619cm^-1的吸收峰归属为Ti—N键,表面吸附了一些有机溶剂,有C=C弯曲振动峰;SEM测试表明其晶粒有立方状、圆粒状,长柱状和内部有中孔的圆环状晶粒,表面存在毛绒状的细小晶须,形成网状包裹在晶粒表面。
TiN nano-powders were synthesized in the stainless steel reaction kettle via solvothermal process at 340℃ for 24h, with xylene as the solvent and the filling ratio of 60% and m (TICl4) : m (NAN3) = 1: 4. The synthesized powders were respectively directly dried, were washed by xylene, anhydrous alcohol and distilled water and then dried at 105 ℃ and were washed by xylene, anhydrous alcohol and distilled water and then calcined at 700 ℃ for 2h. XRD analysis indicate that the prepared TiN3 powders were nano-scale cubic-phase powders, with crystal lattice constant a = 0.4241 nm and average grain size of 11.04 nm. After calcination, the fabricated powders were detected as TiO2 and Ti. IR test revealed that the absorption peak at 619 cm^-1 was detected as Ti-N bond vibration, while the C=C bending vibration resulted from the organic solvent absorption on the surface of the powders was also found. SEM images showed that the micro-morphology of the prepared powders were diversiform, such as cubic grain, round grain, long column and the ring with a center hole inside. On their surfaces there were some tiny crystal whiskers presenting network to coat the crystal surface.