纳米掺N TiO2的制备及光谱分析

以钛酸四丁酯(TBT)及乙二胺(EDA)为前驱体,乙醇为溶剂,冰醋酸为抑制剂,通过溶胶-凝胶法制备了纳米掺NTiO2,并对其结构及光谱性质进行了表征,根据差热-热重分析(TG-DTA)确定了所制备样品的晶型转换温度及最佳的煅烧温度;根据紫外-可见漫反射光谱(UV-Vis/DRS)表征了其光谱吸收特性;根据X射线衍射光谱(XRD)确定了其粒径及晶相结构;根据X射线光电子能谱(XPS)分析了其表面组成。实验考察了光谱吸收带红移程度与乙二胺、钛酸四丁酯的配比及煅烧温度的关系。研究结果表明,制备的纳米掺NTiO2为锐钛矿相,其光谱吸收带发生了明显的红移,乙二胺与钛酸四丁酯的配比及煅烧温度对其光谱吸收有明显的影响。当乙二胺与钛酸四丁酯的摩尔比为1:10,煅烧温度为600℃时,所制备样品对可见光的吸收最强。

Preparation of N-Doped Nanosize TiO2 and Spectral Analysis

Nitrogen-doped nanosize TiO2 was prepared by sol-gel method with TBT and EDA as forerunner body, ethanol as solvent and glacial acetic acid as inhibitor. The crystalline structure and spectrum character were characterzed. According to the curves of differential thermal gravimetric analysis (TG/DTA), the crystal transformation temperature and the best calcining temperature of the obtained samples were determined. According to the ultraviolet-visible diffuse reflection spectrum (UV-Vis/ DRS), the spectral absorption characteristic of the obtained samples was characterized; According to the X-ray diffraction spectrum (XRD), the particle size and crystalline phase structure of the prepared samples were determined; and according to the X-ray photoelectron spectrum (XPS), the superficial composition of the prepared samples was analyzed. The relations between the red shift degree of absorption band and the proportion of EDA/TBT and calcining temperature were investigated in this experiment. The results indicate that the crystal phase of the obtained nitrogen-doped TiO2 is anatase, and the absorption band has a red shift obviously. Both the proportion of EDA/TBT and the calcining temperature have an evident effect on the spectral absorption of the prepared samples. When the mol proportion of EDA/TBT is 1 : 10 and the calcining temperature is 600 degrees C, the spectral absorption of the prepared samples is the strongest.