Electrochemical synthesis, characterization and thermal properties of niobium ethoxide  

作　　者：蔡亚楠 杨声海 金胜明 杨海平 侯国锋 夏姣云 

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

出　　处：《Journal of Central South University》2011年第1期73-77,共5页中南大学学报（英文版）

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

摘　　要：Niobium(V) ethoxide(Nb(OEt)5) was synthesized by electrochemical reaction of ethanol with niobium plate as the sacrificial anode,stainless steel as the cathode and tetraethylammonium chloride(TEAC) as the conductive additive.The condensates were isolated by vacuum distillation under 5 kPa.The product was characterized by Fourier transform infrared(FT-IR) spectra,Raman spectra and nuclear magnetic resonance(NMR) spectra.The results indicate that the product is niobium ethoxide.Thermal properties of niobium ethoxide were analysed by TG/DTG.Vapour pressure was calculated from the Langmuir equation and the enthalpy of vaporization was calculated from the vapour pressure-temperature data using the Clausius-Clapeyron equation.The concentrations of impurity metallic elements in the sample were detected by ICP-MS.It is shown that the purity can reach 99.997%.The volatility and purity of the niobium ethoxide ensure that it could be a good precursor for chemical vapor deposition and atomic layer deposition of niobium oxide layers.Niobium（V） ethoxide （Nb（OEt）5） was synthesized by electrochemical reaction of ethanol with niobium plate as the sacrificial anode, stainless steel as the cathode and tetraethylammonium chloride （TEAC） as the conductive additive. The condensates were isolated by vacuum distillation under 5 kPa. The product was characterized by Fourier transform infrared （FT-IR） spectra, Raman spectra and nuclear magnetic resonance （NMR） spectra. The results indicate that the product is niobium ethoxide. Thermal properties of niobium ethoxide were analysed by TG/DTG. Vapour pressure was calculated from the Langmuir equation and the enthalpy of vaporization was calculated from the vapour pressure-temperature data using the Clausius Clapeyron equation. The concentrations of impurity metallic elements in the sample were detected by ICP-MS. It is shown that the purity can reach 99.997%. The volatility and purity of the niobium ethoxide ensure that it could be a good precursor for chemical vapor deposition and atomic layer deposition of niobium oxide layers.

关 键 词：electrochemical synthesis niobium ethoxide CHARACTERIZATION thermal analysis 

分 类 号：O614.512[理学—无机化学]