溶胶-凝胶法制备高纯钛酸钡粉体的研究  

Study on preparation of high purity barium titanate powder by sol-gel method

作　　者：冯伦伟 刘艳 谢燕[1] FENG Lunwei;LIU Yan;XIE Yan(School of Chemistry and Chemical Engineering,Guizhou University,Guiyang 550025,China)

机构地区：[1]贵州大学化学与化工学院,贵州贵阳550025

出　　处：《无机盐工业》2024年第12期56-61,共6页Inorganic Chemicals Industry

基　　金：贵州省科技重大计划项目(黔科合战略找矿[2022]ZD006)。

摘　　要：钛酸钡在电子工业中应用广泛,被誉为“电子陶瓷工业的支柱”。针对传统溶胶-凝胶法制备钛酸钡多使用有机溶剂和有机金属盐作为原料,存在原料成本高及三废排放等问题。该研究以贵州储量丰富的重晶石矿为原料,重晶石经碳热还原、热水浸取、酸化结晶等步骤制得高纯硝酸钡;再以水为溶剂,采用溶胶-凝胶法,以硝酸钡和无机钛盐为原料通过水解、陈化、蒸发、脱水、焙烧等步骤,制备得到高纯钛酸钡粉体。重点探究了溶胶-凝胶工艺条件对钛酸钡纯度及晶相的影响,获得以水为溶剂的溶胶-凝胶法高纯钛酸钡制备方法;在物料比n(硝酸钡)∶n(硝酸氧钛)∶n(柠檬酸)=1∶1.01∶2、焙烧温度为1100℃、焙烧时间为180 min的最佳工艺条件下,制备所得高纯钛酸钡粉体为四方晶相,主要成分的质量分数达99.85%,满足HG/T 3587—2009《电子工业用高纯钛酸钡》的要求,为重晶石的高价值利用提供了理论和可行性指导。Barium titanate is widely used in the electronics industry and known as“the pillar of the electronic ceramic industry”.The traditional sol-gel method mainly uses organic solvents and organometallic salts as raw materials to prepare barium titanate,which has problems such as high raw material cost and three wastes discharge.In this study,high purity barium nitrate was prepared by carbothermic reduction,hot water leaching,acidification and crystallization of barite from abundant barite ore in Guizhou province.High purity barium titanate powder was prepared by sol-gel method using water as solvent and barium nitrate and inorganic titanium salt as raw materials through hydrolysis,aging,evaporation,dehydration and roasting.The effect of sol-gel process conditions on the purity and crystal phase of barium titanate was focused,and a sol-gel method with water as solvent was obtained to prepare high purity barium titanate.Under the optimum conditions of material ratio n(barium nitrate)∶n(barium nitrate)∶n(citric acid)=1∶1.01∶2,roasting temperature of 1100℃and roasting time of 180 min,the high purity Barium titanate powder was prepared as tetraneous crystal phase with principal component content of 99.85%.The quality met the requirements of HG/T 3587—2009“high purity barium titanate for electronic industry”.This study provided theoretical and feasible guidance for the high value utilization of barite.

关 键 词：重晶石 硝酸钡 溶胶-凝胶法 钛酸钡 

分 类 号：TQ132.35[化学工程—无机化工]