Forming Mechanism of Metal Oxide Thin Films by Liquid Phase Deposition Method

研究了液相沉积法制备金属氧化物薄膜的机理。在研究氧化钛薄膜制备方法的基础上，我们尝试用QCM方法监测氧化钛薄膜在石英晶体上的生长过程。薄膜的沉积速率取决于氟金属配合物和硼酸的浓度，氟金属配合物的平衡反应促成了薄膜的形成反应。根据原位原子力显微镜和原位表面电荷测量，在沉积的诱导阶段，在衬底上观察到氧化物的成核。我们得到了VO_x薄膜，发现薄膜中钒离子的电荷受沉积后加热过程的控制。得到的V_2O_5薄膜在气流中嵌入Li^+离子，并观察到钒离子的电致变色现象。在氮气气流中制备了VO_2薄膜。在约70℃时观察到VO_2薄膜的半导体-金属转变。我们得到了FeOOH和Fe_2O_3薄膜。利用EDTA稀土配合物制备了含稀土金属氧化物薄膜，避免了稀土氟化物的析出。

The forming mechanism of a metal oxide thin film by the liquid phase deposition methods was investigated. Based on the study on the preparation method of the titanium oxide thin film, we tried to monitor the growth process of the thin film on the quartz crystal by QCM method. The deposition rate of the thin film depend on the concentration of fluoro-metal complex and boric acid and the equilibrium reaction of the fluoro-metal complex contributed the film formation reaction. According to in situ AFM and in situ surface charge measurement during the induction period of the deposition, a nucleation of the oxide was observed on the substrate. We obtained VO_x thin films and found that the charge of vanadium ion in the film was controlled by the heating process after deposition. The obtained V_2O_5 film in the air flow intercalated Li^+ ions and the electrochromism phenomenon of the vanadium ion was observed. The VO_2 thin film was obtained in N_2 gas flow. The semiconductor-metal transition of the VO_2 thin film was observed at ca 70。C.We obtained FeOOH and Fe_2O_3 thin films. Also, we succeeded in the preparation of the rare-earth containing metal oxide thin films using the EDTA rare-earth complex in order to avoid the precipitation of the rare-earth fluoride.