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采用钛酸丁酯-水-无水乙醇-盐酸[Ti(OC_4H_9)_4-H_2O-C_2H_5OH-HCl]摩尔比为1:185:10:0.1的体系,以溶胶-凝胶工艺,在溶胶中制备出原位生长的锐铁矿晶体。利用核磁共振仪、扩展X射线吸收精细结构分析、透射电镜对溶胶中的锐钛矿晶体进行深入分析,并考察了锐钛矿晶体的光催化活性。结果表明:前驱体Ti(OC_4H_9)_4完全水解成无机产物。液相中的锐钛矿晶体呈正方体形状,边长约150～200nm。具有与锐钛矿型氧化钛(TiO_2)粉体标样相似的Ti原子K边边前三峰结构,但中心Ti原子与邻近氧原子的配位距离(0.192 1nm)比锐钛矿粉体标样(0.1946nm)的短,Ti原子的配位数(4.18)比锐钛矿粉体标样(6.0)的小。在紫外光照下,所得含有锐钛矿晶体的溶胶可催化降解有机染料罗丹明B(Rhodamine B),15min时对Rhodamine B的降解率达55%:30min时达96%。
The system of Ti (OC 4 H 4) 4 -H 2 O-C 2 H 5 OH-HCl with a molar ratio of 1: 185: 10: 0.1 was prepared by sol-gel process in a sol Out of place growth of anatase crystal. The use of nuclear magnetic resonance spectroscopy, extended X-ray absorption fine structure analysis, transmission electron microscopy anatase crystals in the sol in-depth analysis, and examined the anatase crystal photocatalytic activity. The results show that the precursor Ti (OC_4H_9) _4 is completely hydrolyzed into inorganic products. The anatase crystal in the liquid phase is in the form of a cuboid with a side length of about 150-200 nm. It has the front triplet structure of Ti atom K edge similar to that of anatase titanium dioxide (TiO 2) powder. However, the coordination distance (0.192 1nm) between central Ti atom and adjacent oxygen atom is smaller than that of anatase powder (0.1946nm), the coordination number of Ti atoms (4.18) is smaller than that of anatase powder (6.0). Under UV light, the obtained sol containing anatase crystal could catalyze the degradation of Rhodamine B, which degraded Rhodamine B by 55% at 15 min: 96% at 30 min.