Optimization of parameters, characterization and thermal property analysis of hafnium ethoxide synthesized by electrochemical method

Hafnium ethoxide was synthesized using electrochemical method. Optimization experiments were used to optimize various parameters namely Et4NBr concentration(c): 0.01-0.06 mol/L, solution temperature (t): 30-78 °C, polar distance (D): 2.0-4.0 cm and current density (J): 100-400 A/m2. The electrolytic products obtained under optimum conditions of c=0.04 mol/L, t=78 °C, D=2.0 cm and J=100 A/m2 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 79.1 kJ/mol. The result confirmed that hafnium ethoxide was suitable for the preparation of hafnium oxide by atomic layer deposition.