溶胶-凝胶法制备Ti(C,N)-Mo_2C-Ni复合粉末的研究

Study on Preparation of Ti(C,N)-Mo_2C-Ni Power by Sol-gel Method

本文采用溶胶-凝胶法在较低温度(1 400℃)下制备了Ti(C,N)-Mo2C-Ni金属陶瓷复合粉末。通过红外光谱(FTIR)、X-ray衍射(XRD)、热重分析(TG-DTA),扫描电镜(SEM)、能谱(EDS)、比表面积分析(BET)、氮/氧含量测定等分析检测方法 ,对该粉末的制备过程进行了初步的研究与分析。结果表明:在1 400℃,真空条件下,以钛酸四丁酯为钛源,以蔗糖为碳源,乙二醇为溶剂,采用溶胶-凝胶法结合碳热还原法所制得的Ti(C,N)-Mo2C-Ni金属陶瓷复合粉末晶粒小,纯度较高;其制备机理为:原料通过水解、缩聚、裂解/分解等反应,经过干燥后首先得到TiO2混合先驱体粉末,再经过碳热还原及一系列化学反应最后生成了Ti(C,N)-Mo2C-Ni金属陶瓷复合粉末。

In this research, a kind of Ti（C,N）-Mo2C-Ni cermet powder was prepared by sol-gel method at low temperature （1 400 ℃）. Through infrared spectrum （FTIR）, X-ray ray diffraction （XRD）, thermogravimetric analyzer （TG-DTA）, scanning electron microscopy （SEM）, energy spectrum （EDS）, specific surface area analyzer （BET） and nitrogen/ oxygen content detecting method, the preparation process of the powder was primarily studied and analyzed. The results show that, by using tetrabutyl titanate as titanium source, sucrose as carbon source and ethylene glycol as solvent, the metal ceramic powder prepared by sol-gel method and carbothermal reduction method under the 1 400 ℃ and vacuum conditions, has fine crystal grain and high purity. Its evolution process as that, through hydrolysis, polycondensation, cracking/ decomposition reactions and drying, the TiO2 mixed precursor was obtained, then after carbon thermal reduction and a series of chemical reactions the Ti（C,N）-Mo2C-Ni cermet powder was finally prepared.