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利用四氯化碲与乙醇反应生成前驱体氯代乙醇碲,采用非水解溶胶-凝胶法制备了TeO2凝胶薄膜,通过热处理获得非晶态TeO2薄膜。利用差热分析、X射线衍射和Fourier变换红外光谱等测试手段研究了非水解TeO2的溶胶-凝胶机制、物相变化、以及薄膜制备过程中的析晶现象。结果表明:四氯化碲可与乙醇发生部分亲核取代反应,在非水解溶胶-凝胶体系中生成了含桥氧、桥氯的Te—O—Te和Te—Cl—Te网络结构,凝胶薄膜在热处理过程中有机物碳化和Te—Cl结构的不稳定性易导致Te4+被还原,而对凝胶薄膜煅烧前在200℃进行预烧处理可抑制金属碲的析出,进而获得厚度约150nm、折射率为1.86的TeO2非晶薄膜。
The TeO2 gel film was prepared by the non-hydrolytic sol-gel method using tellurium tetrachloride and ethanol to form the precursor of tellurium chloroethoxide, and the amorphous TeO2 film was obtained by heat treatment. Differential thermal analysis, X-ray diffraction and Fourier transform infrared spectroscopy were used to study the sol-gel mechanism, phase transformation and the crystallization during the preparation of non-hydrolyzed TeO2. The results show that Te 4 Te 4 can react partially with nucleophilic substitution of ethanol, and the network structures of Te-O-Te and Te-Cl-Te containing bridge oxygen and bridged chlorine are formed in the non-hydrolytic sol-gel system. In the process of heat treatment, the carbonization of organic compounds and the instability of Te-Cl structure easily lead to the reduction of Te4 +. Pre-calcination of the gel film at 200 ℃ before calcination can inhibit the precipitation of metal tellurium, The refractive index of 1.86 TeO2 amorphous film.