Ferrites are among the most extensively studied materials, specifically due to their amazing and diverse characteristics. Therefore, we synthesized NixCd1-xAlyFe2-yO4 (NCAF) ferrites using a microwave auto-combustion process, with x varying from 0.0 to 1.0 and y set at 0.1. We conducted a meticulous characterization of their structural, surface morphological, magnetic, molecular vibrational and optical properties. X-ray diffraction confirms the lattice parameter and a single-phase spinel structure. Rietveld refined XRD patterns identified the Fd-3m space group cubic spinel phase. HR-TEM examination shows pseudo-spherical particles with an average size of 40–45 nm. Surface topography exhibits tiny, spherical microstructures. The lognormal histogram showed an average particle size of 56.6 nm–124.8 nm, decreasing with nickel concentration. At a nickel concentration (x) of 0.6, saturation magnetization (Ms) increases and then decreases at 1.0. FTIR confirms no organic phase and spinel development. Absorption measurements determined the band gap energy, which Tauc plot revealed to be 2.5870–2.1657 eV. We used the Kubelka-Munk function to find the band gap energy in the UV–Vis diffuse reflectance spectra (DRS), which was between 2.0027 and 1.6817 eV.