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Zinc oxide (ZnO) is one of the wide-bandgap semiconductors, which may be useful in a plethora of electronic, optical, piezoelectric, and scintillating applications. The following article consists in a structural and luminescence analysis of ZnO microfilms grown on a sapphire substrate with a sol–gel method. The films were annealed at different temperatures. The structures were investigated with the XRD and Raman methods, by which the influence of the substrate on the structure of the film was determined. The luminescence of films was investigated with room-temperature fluorescence, radioluminescence, and thermoluminescence.