利用TeCl_4非水解溶胶-凝胶法制备TeO_2薄膜  

PREPARATION OF TeO_2 THIN FILMS FROM TeCl_4 BY NON-HYDROLYTIC SOL-GEL PROCESSING

作　　者：冯昭彬[1] 林健[1,2] 魏恒勇[1] 李东卫[1] 

机构地区：[1]同济大学材料科学与工程学院,上海200092 [2]同济大学,先进土木工程材料教育部重点实验室,上海200092

出　　处：《硅酸盐学报》2009年第10期1689-1693,共5页Journal of The Chinese Ceramic Society

基　　金：上海市科学技术委员会纳米专项基金(0852nm06500)资助项目

摘　　要：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 precursor（C2H5O）xTeCl4-x was processed by the partial substitution reaction of TeCl4 and C2H5OH.Thin films of TeO2 were prepared by non-hydrolytic sol-gel processing.By using Fourier transform infrared spectroscopy,differential thermal analysis and X-ray diffraction,the transition mechanism of non-hydrolytic sol-gel processing,the phase transformation and the crystallization properties of TeO2 thin film were studied.The results show that a partial nucleophilic substitution reaction takes place between TeCl4 and C2H5OH.The Te—O—Te and Te—Cl—Te networks with the presence of bridging oxygen and bridging chlorine are formed in the non-hydrolytic sol-gel system.Because of the carbonization of organic products in the film and the instability of the Te—Cl structure,Te4＋ tends to be reduced during the calcination of thin films,while the appearance of the crystal can be restrained by pre-heat treatment at 200 ℃ before annealing,and consequently amorphous TeO2 thin films were obtained with t he thickness of 150 nm and refractive index of 1.86.

关 键 词：二氧化碲 薄膜 溶胶-凝胶法 非水解 

分 类 号：TQ171.1[化学工程—玻璃工业]