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 the whole process would decide the quality and reproducible results of YBCO film. In the present report, the barium precursor containing 2,2,6,6-tetramethylheptane-3,5-dionate and tetraethylenepentamine ligands (Ba(TMHD)-tetraen) was synthesized and identified by FTIR, 1H NMR, 13C NMR and ESI-MS spectroscopy. Subsequently the thermal property and the kinetics of decomposition were systematically investigated by combining non-isothermal thermogravimetric analysis methods (TGA), Ozawa, Kissinger and Friedman methods. On the basis of the apparent activation energy of the evaporation process, the thermostability and evaporation characteristics of the precursors were discussed. All results show that Ba(TMHD)-tetraen has higher volatility than Ba(TMHD)2, but it 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)-tetraen breakdown (or thermal aging) during the MOCVD process.
ZHANG Teng, GU Hongwei, DING Fazhu, QU Fei, and DAI Shaotao Key Laboratory of Applied Superconductivity, Institute of Electrical Engineering, Chinese Academy of Sciences, Beijing 100190, China
YBaCuO(YBCO) films with co-doping of Ba Ti O(BTO) and YOnanostructures were successfully fabricated on La Al O(LAO) substrate by metal organic deposition using trifluoroacetates(TFA-MOD). The focus of this study was to optimize the process conditions during the firing heat treatment of high critical current density(J C)-co-doped YBCO films. The effect of the firing temperatures on both the surface morphology and the superconducting properties for the doped YBCO films was systematically studied. According to the X-ray diffraction(XRD) and scanning electron microscopy(SEM) results,the films prepared at 820 and 850 °C show poor electrical performance due to impurity phases and large pores. In contrast, the dense YBCO films prepared at 830 and840 °C with the critical current densities of 10 MA-cm(77 K, 0 T) are obtained.
YBa2Cu3O7-x （YBCO） films with embedded BaZrO3 and BaTiO3 nanoparticles were fabricated by metalorganic deposition using trifluoroacetates （TFA-MOD）. Both X-ray diffraction and transmission electron microscopy revealed that these BaZrO3 and BaTiO3 nanoparticles had random orientations and were distributed stochastically in the YBCO matrix. The unique combined microstructure enhances the critical current density （Jc） of the BaZrO3/BaTiO3 doped-YBCO films, while keeping the critical transition temperature （Tc） close to that in the pure YBCO films. These results indicate that BaZrO3 and BaTiO3 nanoparticles provide strong flux pinning in YBCO films.
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.
Teng ZhangHong-Wei GuFa-Zhu DingFei QuShao-Tao Dai
Owing to the adaptability to large scale processing,excellent composition control and film uniformity,the metal-organic chemical vapor deposition（MOCVD） technique is a promising process for high-temperature superconductor YBa;Cu;O;（YBCO） preparation.In this technique,the 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）copper（II）(Cu（TMHD）;) was synthesized by the interaction of copper acetate hydrate with TMHD in methanol solution,and its structure was identified by FTIR,1 H NMR,and EI-MS spectroscopy.Subsequently,thermal property and the kinetics of decomposition were systematically investigated by nonisothermal thermogravimetric analysis methods（TGA） at different heating rates in streams of N;,and the average apparent activation energy of evaporation process was evaluated by the Ozawa,Kissinger,and Friedman methods.The possible conversion function was estimated through the Coats-Redfern method to characterize the evaporation patterns and followed a phase boundary reaction mechanism by the contracting area equation with average activation energy of 85.1 kJ·mol;.
ZHANG Teng,GU Hongwei,DING Fazhu,QU Fei,and DAI Shaotao Key Laboratory of Applied Superconductivity,Institute of Electrical Engineering,Chinese Academy of Sciences,Beijing 100190,China
In this study, BaTiO3 （BTO）-doped YBCO films are prepared on LaA103 （100） single-crystal substrates by metal- organic decomposition （MOD） using trifluoroacetate （TFA） precursor solutions. The critical current density （Jc） of BTO/YBCO film is as high as 10 MA/cm2 （77 K, 0 T）. The BTO peak is found in the X-ray diffraction （XRD） pattern of a final YBCO superconductivity film. Moreover, a comprehensive study of the precursor evolution is conducted mainly by X-ray analysis and μ-Raman spectroscopy. It is found that the TFA begins to decompose at the beginning of the thermal process, and then further decomposes as temperature increases, and at 700 ℃ BTO nanoparticles begin to appear. It sug- gests that the YBCO film embedded with BTO nanoparticles, whose critical current density （Jc） is enhanced, is successfully prepared by an easily scalable chemical solution deposition technique.
