Sol-Gel, dip-coated titaniumIV and zirconiumIV dioxide monolayered films were deposited on soda-lime glass using titanium and zirconium acetylacetonates as precursors, respectively, and their structural and morphological characterization carried out. The films were heat-treated at different temperatures, 25°C, 150°C, 300°C, and 500°C and, according to Low-angle X-Ray Diffraction analyses (XRD), it was found that TiO2 (anatase) and tetragonal zirconia were present on the substrate, when heated at 500°C. Yoshida and Yajima's method, based on optical information given by the films transmittance UV-Vis spectra, was used to estimate film thickness, refractive index, and, using the Lorentz-Lorentz relationship, their volume fraction. Film thinning and phase formation with increasing temperature was observed, and both titania and zirconia films showed similar behavior during firing. Smooth films with a roughness value of around 2 nm are obtained for the two cases as indicated by Atomic Force Microscopy (AFM) of the surface. Also, formation temperature at around 500°C resulted in the optimum condition to obtain clean stoichiometric TiO2 and ZrO2 thin films on glass substrates as confirmed by X-Ray Photoelectron Spectroscopy (XPS) measurements.