© 2021Design and production of single bilayer ZnO/Al2O3 film have been made by ultrasonically spray pyrolysis technique on glass substrate to develop an alternative high effective photocatalytic material. For detailed evaluation, commonly known comparatives like ZnO, Al2O3, 1%Al:ZnO, and 50%Al:ZnO films have been produced. XRD analyses confirm that films are polycrystalline with hexagonal wurtzite crystal structures. AFM results have been indicated that the variable film morphologies and roughnesses according to film structure. Surface morphologies and thicknesses of the films have been determined via plain view and cross-sectional SEM images. Especially, EDX mapping has been present individually for each layer of ZnO/Al2O3 film and distribution of Zn, Al, O elements, clearly. The calculated optical band gaps of the films have been obtained between 3.11 and 3.63 eV. Photocatalytic activity measurements have been presented an improved photocatalytic performance for ZnO/Al2O3 photocatalyst. Results indicate that photocatalytic activity is correlated with film design.