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本文以钛酸四丁酯、无水乙醇、冰醋酸、硝酸镧和水为原料,通过控制原料配比、反应温度、陈化温度、焙烧温度和焙烧时间,采用溶胶-凝胶法制备了纯的纳米TiO2和四种不同镧掺杂量的TiO2纳米粉体。确定的工艺参数为:原料按照体积比为V水∶V钛酸丁酯∶V无水乙醇∶V冰醋酸=17∶17∶80∶15,凝胶干燥温度选择80℃,粉体焙烧温度为500℃。对所得产物分别采用FT-IR和粉末XRD法进行了表征,FT-IR分析结果表明,掺杂La3+后TiO2的红外吸收峰的位置基本没有发生变化,但部分吸收峰明显宽化,表明掺杂镧引起基团间作用力的改变,使基团的存在环境和键的强弱发生变化,从而导致了红外吸收峰宽化。XRD测试得出所制备的纯TiO2和四种不同镧掺杂量的TiO2粉体的结构均为锐钛矿型TiO2,且随着La掺杂量的增加,TiO2的粒径越来越小,从未掺杂时的26 nm减小到掺杂1%镧时的8 nm,说明镧的掺杂有细化晶粒的作用。
In this paper, tetrabutyl titanate, anhydrous ethanol, glacial acetic acid, lanthanum nitrate and water as raw materials, by controlling the ratio of raw materials, reaction temperature, aging temperature, calcination temperature and calcination time, prepared by sol- Of nano-TiO2 and four different lanthanum doped TiO2 nanopowders. The process parameters are determined as follows: the raw material is V water: V titanate: V anhydrous ethanol: V glacial acetic acid = 17:17:80:15, the gel drying temperature is selected at 80 ° C., the powder calcination temperature is 500 ° C. The results of FT-IR analysis showed that the position of infrared absorption peak of TiO2 after doping La3 + did not change basically, but some of the absorption peaks were obviously widened, which indicated that doping Lanthanum causes the change of the interaction force between the groups, which makes the existence environment of the group and the strength of the bond change, resulting in the broadening of the infrared absorption peak. XRD results show that the pure TiO2 and the four different lanthanum doping TiO2 powders are anatase TiO2. With the increase of La doping amount, the particle size of TiO2 becomes smaller and smaller. The non-doped 26 nm decreases to 8 nm when 1% lanthanum is doped, indicating the effect of lanthanum doping on the grain refinement.