Synthesis, characterization, and thermostability of bis(2,2,6,6-tetramethyl-3, 5-heptanedionato)copper(II)

Abstract

The metal–organic chemical vapor deposition (MOCVD) technique is a promising process for high-temperature superconductor YBa2Cu3O7−δ (YBCO) preparation. In this technique, it is a challenge to obtain barium precursors with high volatility. In addition, the purity, evaporation characteristics, and thermostability of adopted precursors in whole process will decide the quality and reproducible results of YBCO film. In the present report, bis(2,2,6,6-tetramethyl-3,5-heptanedionato)barium(II) (Ba(TMHD)2) was synthesized, and its structure was identified by FTIR, 1H NMR, 13C NMR, and ESI–MS spectroscopy. Subsequently, the thermal properties and the kinetics of decomposition were systematically investigated by nonisothermal thermogravimetric analysis methods. Based on the average apparent activation energy evaluated by the Ozawa, Kissinger, and Friedman methods, the volatilization process was discussed, and all results show that Ba(TMHD)2 is unstable and highly sensitive to the change of temperature during the whole evaporation process. Therefore, it is very important to choose suitable volatilization technology and conditions for avoiding Ba(TMHD)2 breakdown (or thermal aging) during MOCVD process. Subsequently, the possible conversion function is estimated through the Coats–Redfern method to characterize the evaporation patterns and follows a phase boundary reaction mechanism by the contracting surface equation with average activation energy of 118.7 kJ·mol−1. During the metal–organic chemical vapor deposition (MOCVD) process for YBa2Cu3O7−δ preparation, the evaporation characteristics and thermostability of Ba(TMHD)2 will decide the quality and reproducible results of YBCO film. Based on the average apparent activation energy evaluated by the Ozawa, Kissinger, and Friedman methods, the stability of Ba(TMHD)2 can be evaluated by the activation energy changes in evaporation process. All results show that Ba(TMHD)2 is unstable and highly sensitive to the change of temperature during the whole evaporation process.