The Fe and Co single and co-doping effects on the structural and magnetic properties of NiO nanoparticles (NPs) have been studied. The Fe and Co doping into NiO system did not induce any other possible secondary phase (other than NiO) and the average crystallite size was found to be in a narrow range of 33–40 nm which is suitable for studying the doping effects. Room temperature ferromagnetic resonance (FMR) measurements demonstrated the existence of a net magnetization in antiferromagnetic (AFM) NiO NPs which was observed to be increased with an increasing Fe doping and decreasing Co doping concentration. The scattered differential FMR signal for 8% Co doped NiO NPs revealed the presence of randomly oriented magnetic moments in the core of the NPs. However, decreasing the Co doping concentration and increasing the Fe doping concentration increased the degree of homogeneity of the spin structure in the system. The M − H loops taken at room temperature with S-like shape confirmed the presence of a weak ferromagnetism in the Fe doped samples in accordance with FMR analysis and attributed to the double exchange mechanism in these NPs. In ZFC/FC curves, a small peak at low temperatures, in the range of 9–18 K for all the samples, indicates the magnetization contribution from the uncompensated surface spins of these NPs. In addition, a relatively broad peak for higher Fe doping concentrations at higher temperatures indicates the onset of magnetization from the core of these NPs, where Fe and Ni ions may couple parallel or anti-parallel to each other. In summary, Co–Fe co-doping induced a core magnetization in AFM NiO NPs system and makes it attractive for various magnetic applications.