Electrosynthesis, Characterization, and Thermal Property Analysis of Pentakis(Diethylamido)TantaIum

摘要

Pentakis(diethylamido)tantalum (PDEAT) was synthesized by electrochemical reaction involving diethylamide with a sacrificial tantalum anode and stainless steel cathode in the presence of tetraethylammonium bromine as the conductive additive and acetonitrile as the inert support electrolyte. The condensates were isolated by the reduced pressure distillation of as-synthesized crude PDEAT below 5 kPa. The final product was characterized by FT-IR and NMR spectroscopy. The thermal properties of the resulting PDEAT were analyzed by TG-DTG Results indicate that the resulting compound was indeed PDEAT. The vapor pressure of the compound was calculated from the Langmuir equation, while the enthalpy of vaporization was calculated from vapor pressure-temperature data using the Clausius-Clapeyron equation. The concentration of the impurities in the sample were detected via ICP-Mass spectroscopy, and it was found that the purity of the compound synthesized could reach 99.995%.