This study investigates the optical and magnetic properties of nanosized (x)NiO/(1−x)CdFe2O4 (x = 0.1, 0.2, 0.3, 0.4, 0.5, and 1) composites. The samples were synthesized using the wet coprecipitation technique. The X-ray Diffraction patterns demonstrated the formation of Nickel Oxide (NiO) and Cadmium Ferrite (CdFe2O4) phases without any chemical reaction between them. Fourier Transform Infrared results confirm the formation of pure NiO, pure CdFe2O4, and nanosized NiO/CdFe2O4 composites. Transmission Electron Microscopy micrographs show agglomeration between the nanoparticles, demonstrating the magnetic interaction between the oxide and ferrite phases. High-Resolution Transmission Electron Microscopy results verify the presence of NiO and CdFe2O4 phases in each nanosized composite without impurities, which is consistent with the XRD data. The ultraviolet–visible spectroscopy results confirmed that HCl is a better solvent than ethanol in investigating the optical properties of nanosized oxide/ferrite composites. Photoluminescence spectra exhibited asymmetricity owing to the presence of various emission peaks, which reveals the distribution of defect states within the bandgap of the nanosized composites. The Mössbauer spectra of the nanosized composites comprised an asymmetrical doublet at 300 K and an asymmetrical centered doublet within minor sextets at 77 K. Vibrating Sample Magnetometer study showed a shift at 77 K, which can be attributed to the spontaneous exchange bias effect. The magnetic parameters extracted from the M − H loops of all the synthesized nanosized composites at 77 K are higher than those at 300 K.