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溶剂热合成纳米氮化钛粉体的研究
Solvothermal Synthesis of Titanium Nitride Nanopowders
【摘要】 将质量比为1:4的TiCl4和NaN3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α=0.4241nm,平均粒径为11.04 nm,700℃煅烧后全部转化为TiO2和Ti的混合物;IR测试表明在619 cm-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。
【Abstract】 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-1was 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.
- 【文献出处】 稀有金属材料与工程 ,Rare Metal Materials and Engineering , 编辑部邮箱 ,2007年S2期
- 【分类号】O614.411
- 【被引频次】20
- 【下载频次】379