块状TiO2气凝胶的制备及其表征

随着以溶胶-凝胶法和超临界干燥技术为基础的气凝胶制备方法的逐步完善,已不断制备出多种气凝胶1～3].由于TiO2具有半导体特性,它常被作为光催化剂而受到重视,但是TiO2气凝胶的结构强度远比SiO2气凝胶小,在制备过程中极易碎裂粉化,所以至今未见制备块状TiO2气凝胶的报道.Dagan等4]曾用异钛酸丁酯为母体制得TiO2气凝胶,并发现水杨酸在TiO2气凝胶存在下的光解速率是一般TiO2粉末的10倍,但获得的仅为TiO2气凝胶粉末.张敬畅等5]以无机盐为原料,采用溶胶-凝胶法结合超临界干燥技术制备了纳米级TiO2气凝胶,也未能得到块状TiO2气凝胶材料. 本文报道以正钛酸丁酯为原料制备块状TiO2气凝胶的方法,并用TEM,SEM,XRD和IR等手段对所获得的气凝胶进行了结构表征.

Preparation and Characterization of Monolithic TiO2 Aerogels

Monolithic TiO₂ aerogels have been prepared from titanium n butoxide by sol-gel process and supercritical drying technique, and the structural properties of the aerogel samples have been characterized by means of SEM, TEM, XRD, IR, BETand pore distribution analysis. The results indicated that the optimum condition for preparing monolithic TiO₂ aerogels was n-Ti(OC₄H₉)₄]: n-(C₂H₅OH): n-(H₂O): n-(HNO₃)=1:18.3:3.75:0.14. The final aerogels which consist of colloidal particles with diameters of about 5 nm were found to be with coherent uniform size and low density solid inorganic materials with porosity of about 90%, and contained mesopore in the range of 10-20 nm. The monolithic TiO₂ aerogels were of the pure amorphous form at room temperature, which would be converted into anatase and then into rutile by increasing the temperature of heat treatment.