Phase separation in SiO2–TiO2 gel and glassy films studied by atomic force microscopy and transmission electron microscopy

An investigation of phase separation phenomena in gel and glassy thin films of silica–titania, with TiO2 contents of 20 and 40 mol%, has been carried out by atomic force microscopy (AFM) and transmission electron microscopy (TEM). The thin films were prepared by spin coating of a precursor sol on silicon wafers. Both the TEM measurements (carried out on scrapped thin film flakes) and the AFM measurements (carried out on films coated on the silicon substrates) for samples with different heat treatments suggest that spinodal-like structural inhomogeneities occur in these samples, unlike the corresponding observations in pure silica films, which are known to be homogeneous. Changes in the microstructure of the films have been noticed with the thermal treatment, in agreement with earlier x-ray photoemission studies. The finer characteristic dimensions of the phase separated regions reveal that silica–titania samples prepared by sol-gel processing exhibit a more intimate mixing of the phases.