The structural, magnetic, and electronic structural properties of Ni0.2Cd0.3Fe(2.5-x)Al(x)O4 ferrite nanoparticles were studied via X-ray diffraction (XRD), transmission electron microscopy (TEM), DC magnetization, and near-edge X-ray absorption fine-structure spectroscopy (NEXAFS) measurements. Nanoparticles of Ni0.2Cd0.3Fe(2.5x)Al(x)O4 (0 < or = x < or = 0.4) ferrite were synthesized using the sol-gel method. The XRD and TEM measurements showed that all the samples had a single-phase nature with a cubic structure, and had nanocrystalline behavior. From the XRD and TEM analysis, it was found that the particle size increases with Al doping. The DC magnetization measurements revealed that the blocking temperature increases with increased Al doping. It was observed that the magnetic moment decreases with Al doping, which may be due to the dilution of the sublattice by the doping of the Al ions. The NEXAFS measurements performed at room temperature indicated that Fe exists in a mixed-valence state.