电化学合成乙醇铪的参数优化、表征和热性能分析.pdf

Trans.NonferrousMet.Soc.China27(2017) 694−700 Optimization ofparameters,characterization andthermalproperty analysisof hafnium ethoxide synthesizedby electrochemicalmethod Chang-hongWANG,Sheng-haiYANG,Yong-ming CHEN,Yan-zengWU,JingHE,Chao-boTANG SchoolofMetallurgy andEnvironment,Central South University,Changsha410083,China Received2February 2016;accepted 15June2016 Abstract: Hafnium ethoxide was synthesized using electrochemical method. Optimization experiments were used to optimize various parameters namely Et NBr concentration(c): 0.01−0.06 mol/L, solution temperature (t): 30−78 °C, polar distance (D): 4 2 2.0−4.0 cm and current density (J): 100−400A/m . The electrolytic products obtained under optimum conditions of c 0.04 mol/L, 2 t 78 °C, D 2.0 cm and J 100 A/m were further isolated by vacuum distillation under 5 kPa. The product was characterized by Fourier transform infrared (FT-IR) spectra, nuclear magnetic resonance (NMR) spectra. The results indicated that the product was hafnium ethoxide. ICP analysis suggested that the content of hafnium ethoxide in the final product exceeded 99.997%. Thermal properties of the product were analyzed by TG/DTG. The vaporization enthalpy of hafnium ethoxide was found to be 79.1kJ/mol. Theresult confirmedthathafnium ethoxidewassuitableforthepreparation ofhafnium oxideby atomic layer deposition. Key words:hafnium ethoxide;electrochemical synthesis;parameter optimization;characterization;thermal analysis the environment. In addition, the necessary reagents are 1Introduction scarce and the reactions involve various side process