The challenge of producing cost-effective oxygen electrocatalysts for the oxygen reduction reaction (ORR) continues to impede the advancement of fuel cell technology. Herein, we report the effect of Ni and activated carbon on mixed metal (Ni,Fe)Co2O4 and (Ni,Fe)Co2O4@C spinel oxide nanoparticles synthesized by facile and versatile co-precipitation method followed by the physio-chemical, morphological properties and electrochemical analysis towards oxygen reduction reaction. The formation of FeCo2O4, (Ni,Fe)Co2O4 and (Ni,Fe)Co2O4@C nanoparticles was confirmed with X-ray diffraction and Raman analysis while D and G band revealed the presence of carbon in the (Ni,Fe)Co2O4@C nanoparticles. The Brunauer–Emmett–Teller analysis reveals the mesoporous behaviour of the synthesized multi-metal oxide nanoparticles. X-ray photoelectron spectroscopy analysis reveals the presence of Co3+/Co2+, Fe3+/Fe2+, Ni3+/Ni2+, O1s and C1s confirms the formation of complex (Fe3+Co2+)(Ni2+Ni3+Fe2+Fe3+Co3+)2O4 spinel structure. The ionic radii of the Co, Fe and Ni ions plays a vital role in the formation of complex spinel structures. The ORR analysis was studied by electrochemical analysis and observed (Ni,Fe)Co2O4 outperformed FeCo2O4 in terms of onset potential and current densities for the ORR. (Ni,Fe)Co2O4@C exhibited the highest catalytic activity with −2.18 mAcm−2 at 0.1 V vs RHE, which is relatively comparable with that of commercial Pt/C. Furthermore, the electrocatalytic analysis revealed the ORR mechanism adheres to the direct "4e−" process. The intermetallic interactions between the Co, Fe and Ni ions along with high crystallinity, significant surface area, high porosity, and the influence of carbon incorporation that are all contribute to the improved electrocatalytic activity of the cobalite-based multi-metal spinel oxides.