Rm. Almeida et Ee. Christensen, CRYSTALLIZATION BEHAVIOR OF SIO2-TIO2 SOL-GEL THIN-FILMS, JOURNAL OF SOL-GEL SCIENCE AND TECHNOLOGY, 8(1-3), 1997, pp. 409-413
The aim of this work was to investigate the crystallization behavior o
f thin films of SiO2-TiO2 made by the sol-gel process as function of d
ie TiO2 content and the temperature and time of heat treatment. Precur
sor solutions were prepared by hydrolysis of TEOS (tetraethoxysilane)
and TPOT (titanium tetraisopropoxide). Multilayer films were spun on s
ingle crystal silicon wafers. The compositions studied were (on a mola
r percentage basis) 20TiO(2)-80SiO(2), 30TiO(2)-70SiO(2), 40TiO(2)-60S
iO(2) and pure TiO2. The films were heat treated at different temperat
ures between 300 degrees C and 1200 degrees C, for different periods o
f time (30 s-90 h). The crystallization kinetics were followed by micr
o-Raman spectrometry. Grazing incidence X-ray diffraction showed that
the films crystallized into one or both of two crystalline phases of T
iO2: anatase and rutile (for pure TiO2 only). The volume fractions of
the crystalline phase varied from very low values (<1%), up to 100%, f
or a TiO2 sample heat treated at 800 degrees C for 8 hours. The result
s show that the volume fraction of crystalline phase is strongly influ
enced by the heat treatment temperature and also, to a smaller extent,
by the heat treatment time. The most important parameter, however, is
the composition of the films: the higher their TiO2 concentration, th
e lower is the crystallization temperature and the larger is the cryst
allized fraction.