在乙二醇甲醚溶液中电解合成ZnTiO_3超细粉末  

Synthesis of Nano-sized Particle Spinel ZnTiO_3 by Electrolysis in CH_3OCH_2CH_2OH Solution

作　　者：朱传高[1] 王凤武[1] 徐迈[1] 方文彦[1] 

机构地区：[1]淮南师范学院化学系,淮南232001

出　　处：《硅酸盐通报》2011年第1期210-215,共6页Bulletin of the Chinese Ceramic Society

基　　金：安徽省自然科学基金重点项目(KJ2010A309;KJ2009A47)

摘　　要：在无隔膜电解槽中,加入0.035 mol·dm-3（Bu4N）B r的乙二醇甲醚溶液,保持电解温度30℃、电流密度30mA·cm-2,先电解钛片6 h,再电解锌片3 h,制得锌、钛醇盐配合物ZnTi（OCH2CH2OCH3）6,电流效率为95.4%。采用红外、拉曼光谱对其进行了表征。结果表明,前驱体中含有配体（OCH2CH2OCH3）6,可以有效克服团聚现象。水解后干燥24 h得到干凝胶,在450℃煅烧2 h制得纳米ZnTiO3粉体。经X射线衍射、电子透射显微镜测试表明,干凝胶粒径为25 nm,钛酸锌粒径在20~30 nm,纯度较高。Zinc and titanium alkoxide was prepared in the cell without diaphragm when the titanium sheet was electrolysed for 6 h and then zinc sheet was electrolysed for 3 h tetrabutylammonium（0.035 mol·dm-3） bromides were added to serve as supporting electrolyte.Glycol and methyl ether were used as electrolyte.Current density of 30 A·dm-2 and temperature of 30 ℃were employed.The current efficiency was 95.4%.The structure of precursor was analyzed by laser Raman spectra,infrared spectroscopy.The xerogel was prepared by vacuum drying for 24 h after hydrolyzi.The obtained xerogel were calcined at 450 ℃,2 h in air.After 2 h,the nano ZnTiO3 were prepared successfully.The structural characterization of the xerogeld and nano ZnTiO3 was performed by X-ray diffraction（XRD）,transmission electron microscopy（TEM）.The results indicated that ZnTiO3 nano-particles（size 20-30 nm） are obtained.The grain of xerogel was about 25 nm.The product is high purity.

关 键 词：电解 锌、钛配合物 溶胶-凝胶 纳米ZnTiO3 

分 类 号：TF12[冶金工程—粉末冶金]