Silica and silica-titania glasses prepared by the sol-gel process

Clear monolithic samples of silica and silica-titania glasses were prepared by the sol-gel process from alkoxides as starting materials. The effects of the composition of the initial alcoholic solutions on the gelation of the silica materials and the effects of using different titanium compounds on the formation of silica-titania gels and glasses were investigated. DTA and TGA revealed losses of water and organic volatiles during heat treatment of the gels at lower temperatures (up to 400°C) and the glass transformation and crystallization behaviour at higher temperatures (up to 1500°C). The effects of using atmospheres with varying oxygen contents on the DTA peaks caused by oxidation reactions were also studied. Structural changes occurring during heat treatment were monitored by infra-red spectroscopy which indicated that the water contents of the glasses after heat treatment to 900°C were about 1000 ppm. Transmission electron microscopy of ion beam thinned foils of a 80 SiO 220TiO 2 composition showed a microstructure of extremely fine pores for heat treatments up to 1000°C. However, after extended heat treatments above 950–1000°C, the porosity appeared to decrease and a high concentration of fine crystallites of anatase (approximately 100 Å in diameter) embedded in a silica-rich glass matrix were obtained.