Mixed oxides have received remarkable attention due to the many opportunities to adjust their interesting structural, electrical, catalytic properties, leading to a better, more useful performance compared to the basic metal oxides. In this study, mixed oxides NiO/ZnO/Al2O3 were synthesized in a single step via the ultrasonic spray pyrolysis method using nitrate salts, and the temperature effects of the process were investigated (400, 600, 800 °C). The synthesized samples were characterized by means of scanning electron microscopy, energy-dispersive spectroscopy, X-ray diffraction and Raman spectroscopy analyses. The results showed Al2O3, NiO–Al2O3 and ZnO–Al2O3 systems with spinel phases. Furthermore, the Raman peaks supported the coexistence of oxide phases, which strongly impact the overall properties of nanocomposite.