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The effect of Fe and Mn co-doping on the magnetic properties of the antiferromagnetic (AFM) NiO nanoparticles which offer large potential for different magnetic applications have been studied. The Rietveld refinement fitting of powder x-ray diffractometry (XRD) patterns confirmed the phase formation of face-centred cubic crystal structure of NiO and average crystallite size lies in the short range of 32–38 nm. The cavity and broadband ferromagnetic resonance (FMR) measurements taken at room temperature demonstrate the smaller local magnetic inhomogeneity for 4%Mn-4%Fe co-doped NiO nanoparticles as compared to undoped, single doped and co-doped with different concentration NiO nanoparticles. The M-H loops revealed the room temperature ferromagnetism-like behaviour for higher Fe doping concentration and lower Mn doping concentration. This can be attributed to the double exchange interaction. The zero field cooled (ZFC) and field cooled (FC) dc magnetization curves showed a small surface freezing peak (at at low temperatures and a blocking peak (at at higher temperatures. For samples with 4%Mn-4%Fe and 2%Mn-6%Fe, the blocking peak was found at a relatively high temperature in comparison to other samples. This can be attributed to the presence of magnetic exchange interactions which block the magnetic spins against a thermal increase. The ZFC AC-susceptibility showed three peaks; a surface freezing peak at Tf, a blocking peak at TB peak and an anomalous peak at Tx in between and , which was found to be most prominent for the 4%Mn-4%Fe co-doped nanoparticles. The neutron diffraction pattern confirmed the AFM order of the core of the 4%Mn-4%Fe co-doped nanoparticles, which indicates an AFM coupling between the Fe2+ and Mn2+ ions and the Ni2+ ions through super-exchange interaction. Therefore, the origin of TX peak can be attributed to the ferromagnetic coupling between the Fe2+ and Mn2+ ions which has a maximum strength at equal concentration. Thus, small and equal doping concentration of Fe and Mn in NiO nanoparticles increase the magnetic homogeneity which makes them attractive for magnetic applications.