ZnAl 2 O 4 /ZnO nanocomposites with different ZnO (20,30, and 40 mol%) concentrations and coated samples on supports were successfully prepared through combustion synthesis assisted by microwave. Two catalyst supports (a-Al 2 O 3 granules and c-Al 2 O 3 granules) in the forming of granules were used by sintering. The obtained products after calcination were characterized by X-ray diffraction (XRD), electron microscopy (SEM and TEM), Brunauer-Emmett-Teller (BET), dynamic light scattering (DLS), photoluminescence spectroscopy (PL), and UV-Vis spectroscopy. Samples were studied by degradation of methyl orange (MO) under UV irradiation in a photoreactor to evaluate the photocatalytic performance. Degradation using a ZnAl 2 O 4 /ZnO (30 mol%) nanocomposite reached 97.1 %. cAl 2 O 3 granules have demonstrated considerable difference in photocatalytic efficiency compared to a-Al 2 O 3 granules. Therefore, the coated granules were able to & Mozhgan Shahmirzaee be employed for the removal of dyes from wastewater, having desirable repeatability and reusability. Our results may initiate large-scale production of coated layers with promising photocatalytic performances.