电化学方法制备纳米MgTiO_3及表征  

Preparation and characterization of nano-sized MgTiO_3 powder by sacrificial anode

作　　者：陈永红[1] 朱传高[1] 魏亦军[1] 褚道葆[2] 

机构地区：[1]淮南师范学院实验信息中心,淮南232001 [2]安徽师范大学有机化学研究所,芜湖241000

出　　处：《化工新型材料》2005年第5期41-43,3,共4页New Chemical Materials

基　　金：安徽省教育厅自然科学基金资助项目(No.2004kj326)

摘　　要：以金属阳极溶解法制得MgTiO3前驱体MgTi(OCH2CH3)(6-y)(acac)y[acac为乙酰丙酮基];讨论了影响电合成镁、钛醇盐配合物的主要因素。在pH=8.5的条件下,将含有前驱体的电解液直接水解形成凝胶,凝胶经洗涤、干燥后,在500℃下煅烧2h,制得纳米Mg-TiO3粉体。采用红外(IR)、热重-差热分析(TG-DTA)、X-射线衍射(XRD)、电子透射技术(TEM)等对前驱体和纳米Mg-TiO3进行了表征。实验表明,在使用导电盐Bu4NBr浓度0.04mol/L,控制电解液温度35～40℃之间的条件下,制得的纳米Mg-TiO3粉体纯度高,平均粒径在20～30nm之间。The precursor MgTi(OCH_2CH_3)_((6-y))(acac)y of the mixed oxide MgTiO_3 was synthesized by electrochemical dissolution of titanium in ethanol and acetylacetone solution. The factors such as temperature and concentration of conductive additive influencing current efficiency and product yield were also investigated. The nano-powder MgTiO_3 was prepared by a direct sol-gel process of the electrolyte solution under pH=8.5, lavation and calcinations for 2h at 500℃. IR. spectrum, XRD, and TEM were used to characterize the structure of nano-sized MgTiO_3 and its precursor. The results turned out that the temperature controlled between 35～40℃, and concentration of conductive additive Bu_4NBr of 0.04mol/L could improve current efficiency and electrolysis yield, and nano-sized MgTiO_3 with a narrow size distribution of 20~30 nm was obtained, which had a high purity. This process may be recommended as a promising method to synthesize the other nano-oxides.

关 键 词：MGTIO3 电化学方法 纳米 表征 热重-差热分析 制备 X-射线衍射 电解液温度 前驱体 阳极溶解 电子透射 平均粒径 电合成 配合物 钛醇盐 500 凝胶 粉体 水解 煅烧 

分 类 号：O614[理学—无机化学]