Electrochemical synthesis and characterization of tantalum alkoxides
(1. School of Metallurgical Science and Engineering, Central South University, Changsha 410083, China;
2. School of Minerals Processing and Bioengineering, Central South University, Changsha 410083, China)
2. School of Minerals Processing and Bioengineering, Central South University, Changsha 410083, China)
Abstract: Tantalum(Ⅴ) propoxide (Ta(OPrn)5), isopropoxide (Ta(OPri)5) and butoxide(Ta(OBun)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.
Key words: electrochemical synthesis; tantalum alkoxides; spectral characterization; thermal analysis