The semiconductor-transition conducting metal oxides (p-type NiO: n-type ZnO) nanocomposites (NCs) called (NZO) are successfully prepared by a simple wet-chemical route followed by the systematic sintering at different temperatures such as 400°C, 500°C, 600°C, and 700 °C. The structure and morphology of the samples were characterized by X-ray diffraction (XRD), high-resolution scanning/transmission electron microscopy (HR-SEM/TEM), and energy-dispersive X-ray spectrometry (EDX) techniques. XRD analysis reveals that the average crystallite size of the NZO NCs was found to be in the range 16-18 nm. The synthesized sample discloses a ferromagnetic behavior. The photocatalytic degradation of rhodamine B in an aqueous solution was superior at the NZO NC at 600 °C in comparison with other samples. Here, the NZO NCs display to be good candidates for magnetic and photocatalytic application.