Electrochemical synthesis and characterization of tantalum alkoxides  

作　　者：杨声海 蔡亚楠 杨海平 金胜明 

机构地区：[1]School of Metallurgical Science and Engineering,Central South University [2]School of Minerals Processing and Bioengineering,Central South University

出　　处：《中国有色金属学会会刊：英文版》2009年第6期1504-1508,共5页Transactions of Nonferrous Metals Society of China

基　　金：Project(2007AA03Z425)supported by the Hi-tech Research and Development Program of China;Project(50404011)supported by the National Natural Science Foundation of China

摘　　要：Tantalum(Ⅴ)propoxide(Ta(OPrn)5),isopropoxide(Ta(OPr i )5)and butoxide(Ta(OBu n )5)were synthesized by electro- chemical reactions of corresponding alcohol at sacrificial tantalum anode in the presence of tetraethylammonium chloride as a conductive additive.The pure products were isolated by reduced pressure distillation under 5 kPa.The crystal of Ta(OPri)5 was obtained by recrystallization from hexane at-10℃.These samples were characterized by Fourier transform infrared spectra(FT-IR), Raman spectra,nuclear magnetic resonance spectra(NMR),TG/DTA and ICP-MS.The results show that direct electrochemical synthesis of metal alkoxides has a high current efficiency and electrolysis yield.These alkoxides have a high purity of 99.97%and can be directly used as the precursor of Ta2O5 films.Tantalum（V） propoxide （Ta（OPr^n）5）, isopropoxide （Ta（OPr^i）5） and butoxide（Ta（OBu^n）5） were synthesized by electrochemical reactions of corresponding alcohol at sacrificial tantalum anode in the presence of tetraethylammonium chloride as a conductive additive. The pure products were isolated by reduced pressure distillation under 5 kPa. The crystal of Ta（OPr^i）5 was obtained by recrystallization from hexane at -10 ℃. These samples were characterized by Fourier transform infrared spectra （FT-IR）, Raman spectra, nuclear magnetic resonance spectra （NMR）, TG/DTA and ICP-MS. The results show that direct electrochemical synthesis of metal alkoxides has a high current efficiency and electrolysis yield. These alkoxides have a high purity of 99.97% and can be directly used as the precursor of Ta2O5 films.

关 键 词：直接电化学合成 金属醇盐 钽薄膜 傅立叶变换红外光谱 表征 核磁共振谱 导电添加剂 电化学反应 

分 类 号：O611.3[理学—无机化学]