非水解溶胶-凝胶碳热还原氮化法制备TiN粉体工艺研究  

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

作　　者：刘会兴 魏恒勇[1,2] 崔燚 卜景龙[1,2] 魏颖娜 张璞[3] 张利芳 

机构地区：[1]河北联合大学材料科学与工程学院,唐山063009 [2]河北省无机非金属材料重点实验室,唐山063009 [3]中国轻工业陶瓷研究所,景德镇333000

出　　处：《中国陶瓷》2015年第6期10-14,共5页China Ceramics

基　　金：国家自然科学基金(51272066);河北省自然科学基金(E2013209183)

摘　　要：以四氯化钛和异丙醚为原料,二氯甲烷为溶剂,以非水解溶胶-凝胶法制备的Ti O2凝胶为钛源,选用分子量为1300000的聚乙烯吡咯烷酮(PVP)为碳源,采用碳热还原氮化法合成Ti N粉体。通过XRD和FE-SEM研究了PVP用量、合成温度及保温时间、氮气流量对Ti N粉体合成的影响。结果表明,适当增加PVP用量有助于Ti N的合成,但残余游离碳也相应增多;氮气流量一定时,升高合成温度及延长保温时间,有利于Ti N粉体纯度的提高,残余的游离碳变少,晶胞参数接近于标准值;当合成温度为1300℃,保温时间为5 h,氮气流量为40 m L/min时,制备出的Ti N粉体纯度高,晶粒发育良好,形状近似球形,粒径约为0.4μm。Titanium dioxide gel precursor was prepared by non-hydrolytic sol-gel method using titanium tetrachloride and isopropyl ether as raw materials,dichloromethane as solvent,respectively.The Ti N powers were synthesized via carbon thermal reduction nitridation method using the non-hydrolytic Ti O2 gel as titanium source and polyvinylpyrrolidone(molecular weight 1300000) as carbon source,respectively.The effects of polyvinylpyrrolidone(PVP) dosage,synthesis temperature and soaking time,nitrogen gas flow on the synthesis of Ti N powders were studied by XRD and FE-SEM.The results show that appropriate increase dosage of PVP could improve the synthesis of Ti N powders.When the nitrogen gas flow was determined,synthesis temperature and holding time were increased,the purity of Ti N powers was increased with their crystal cell parameters closer to the standard values,and the residual free carbon were reduced.When synthesis temperature was 1300 ℃,holding time was 5 h and N2 flux was 40 m L/min,high purity Ti N powders were prepared,and their particle shape was spherical approximately with particle size of about 0.4 μm.

关 键 词：非水解溶胶-凝胶 碳热还原氮化 TI N粉体 

分 类 号：TQ174.61[化学工程—陶瓷工业]