摘要
以廉价的TiCl4为原料,液体石蜡为纯化剂,氨水作形核剂,制备出高纯TiO2超微粉体。用XRF分析了样品的物相组成;XRD和SEM等手段表征了粉体合成过程的物相变化和形貌特征。结果表明,TiCl4经过矿物油(液体石蜡)除钒和精馏除铁等杂质后进行水解,当TiCl4溶液浓度0.65 mol/L,水解温度60℃、反应时间2 h、pH值=7、在800℃煅烧2 h条件下,制备出TiO2的纯度达到99.9952%,晶型为金红石相,晶粒尺寸约0.65μm,形貌近球形。
The high-purity TiO2 ultra-fine powders were prepared by TiCl4 hydrolysis using low-cost TiCl4 as raw materials,liquid olefin as purifier and NH3· H2O as nucleation agent.The phase composition of the sample was analyzed by XRF;The phase transformation and morphology character of the powders were studied by XRD and SEM during preparation of TiO2 particles.The results indicated that TiCl4 was purified by liquid olefin in order to wipe off vanadium,in the meantime removed iron by the method of rectification,after which TiCl4 was forced to proceed a hydrolysis reaction.The powders whose purity is 99.9952% are approximately 650 nm spherical particles with good and crystalline phase is rutile under the condition of n(Ti4+)=0.65 mol/L,pH=7,treated at 60 ℃ for 2 h and calcined at 800 ℃ for 2 h.
出处
《人工晶体学报》
EI
CAS
CSCD
北大核心
2012年第2期485-490,共6页
Journal of Synthetic Crystals
基金
辽宁省教育厅重点实验室项目(20008S181)
沈阳市科技攻关计划项目(F10-053-2-00)
关键词
TIO2
物相变化
水解法
金红石相
TiO2
phase transformation
hydrolysis method
rutile phase