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Zinc oxide films were fabricated by a home-made spray pyrolysis system equipped with an optical set-up ensuring the in-situ control of the film growth 0.1 M of zinc acetate diluted in a mixture of ethanol and water was used as the precursor solution. The deposition temperature and the pH of the precursor solution were kept at 350°C and 4.5, respectively. X-ray diffraction patterns revealed that films were zincite-like with a grain size depending of the ethanol/water molar ratio, Γ, in the precursor solution. The interference pattern obtained during film deposition was used to monito the film roughness: it was found that this is related with those results of surfaces and optical analysis obtained by scanning electron microscopy (SEM) and spectrophotometric measurements, respectively. Photo-electrocatalytic results indicated that there is a correlation of the partial molar volume of etha...