Journal of Thermal Analysis and Calorimetry p. 37 - 46 (2001)
Update date:2022-08-31
Topics:
Ingo
Riccucci
Bultrini
Dire
Chiozzini
Amorphous SiO2, TiO2 and xSiO2-(1-x)TiO2 ceramic materials with selected values of x 0.5, 0.7 and 0.9, have been prepared via sol-gel process using silicon tetraethoxysilane (TEOS) and titanium tetraisopropoxide Ti(OPri)4. By means of the combined use of differential thermal analysis (DTA), thermogravimetry (TG), X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photo-electron spectroscopy (XPS) and X-ray induced Auger electron spectroscopy (XAES), the surface microchemical structure and morphology of the sol-gel materials have been studied as a function of thermal treatments carried out in air up to 1200°C. In the range of temperature from 50 to 450°C, DTA-TG results evidence a remarkable mass loss due to the evaporation of organic solvents entrapped in the sol-gel materials and of the remnant organic components of the precursor metal alkoxides. In the range of temperature from 400 to about 1000°C, by means of the combined use of DTA, XRD, XPS and XAES techniques as a function of temperature and of chemical composition, it is possible to evidence the formation of crystalline phases such as quartz, anatase and rutile. Furthermore, lineshape analysis of O 1s XPS peak allows to distinguish between single O-Ti and O-Si bonds and also to disclose the presence of cross linking Si-O-Ti bonds, that act as bridges between SiO2 and TiO2 moieties. As a function of temperature, Si-O-Ti bonds are broken and the formation of new Ti-O and Si-O bonds as in TiO2 and SiO2 takes place as well as a silica segregation phenomenon.
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