Electrochemical synthesis and characterization of tantalum alkoxides

Tantalum(V) propoxide (Ta(OPrn)5), isopropoxide (Ta(OPri)5) and butoxide(Ta(OBun)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(OPri)5 was obtained by recrystallization from hexane at −10 °C. 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.