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Synthesis, characterization, and thermostability of bis(2,2,6,6-tetramethyl-3,5-heptanedionato)barium(Ⅱ) 被引量:1

Synthesis, characterization, and thermostability of bis(2,2,6,6-tetramethyl-3,5-heptanedionato)barium(Ⅱ)
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摘要 The metal-organic chemical vapor deposition (MOCVD) technique is a promising process for high-tem- perature superconductor YBa2Cu307_6(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 synthe- sized, and its structure was identified by PTIR, 1H NMR, 13C NMR, and ESI-MS spectroscopy. Subsequently, the thermal properties and the kinetics of decomposition were systemati- cally investigated by nonisothermal thermogravimetric anal- ysis 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. There- fore, it is very important to choose suitable volatilization technology and conditions for avoiding Ba(TMHD)2 break- down (or thermal aging) during MOCVD process. Subse- quently, 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.mo1-1. The metal-organic chemical vapor deposition (MOCVD) technique is a promising process for high-tem- perature superconductor YBa2Cu307_6(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 synthe- sized, and its structure was identified by PTIR, 1H NMR, 13C NMR, and ESI-MS spectroscopy. Subsequently, the thermal properties and the kinetics of decomposition were systemati- cally investigated by nonisothermal thermogravimetric anal- ysis 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. There- fore, it is very important to choose suitable volatilization technology and conditions for avoiding Ba(TMHD)2 break- down (or thermal aging) during MOCVD process. Subse- quently, 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.mo1-1.
出处 《Rare Metals》 SCIE EI CAS CSCD 2013年第1期67-74,共8页 稀有金属(英文版)
基金 financially supported by the Major State Basic Research Development Program of China(No.2011CBA00105) the National Natural Science Foundation of China(Nos.51002149 and 21101151)
关键词 Ba(TMHD)2 Metal-organic chemical vapordeposition (MOCVD) SYNTHESIS Thermostability Ba(TMHD)2 Metal-organic chemical vapordeposition (MOCVD) Synthesis Thermostability
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