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.
出处
《硅酸盐通报》
CAS
CSCD
北大核心
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)