Enormous efforts have been dedicated to engineering low-cost and efficient electrocatalysts for both hydrogen evolution and oxygen evolution reactions (HER and OER, respectively). For this, the current contribution reports the successful synthesis of binary/ternary metal ferrites (Co x Ni 1−x Ferrite; x = 0.0, 0.1, 0.3, 0.5, 0.7, and 1.0) by a simple one-step microwave technique and subsequently discusses its chemical and electrochemical properties. The X-ray diffraction analysis substantiated the phase purity of the as-obtained catalysts with various compositions. Additionally, the morphology of the nanoparticles was identified via transmission electron microscopy. Further, the vibrating sample magnetometer justified the ferromagnetic character of the as-prepared products. The electrochemical measurements revealed that the as-prepared materials required the overpotentials of 422−600 and 419−467 mV for HER and OER, respectively, to afford current densities of 10 mA cm −2 . In the general sense, Ni cation substitution with Co influenced favorably toward both HER and OER. Among all synthesized electrocatalysts, Co 0.9 Ni 0.1 Ferrite displayed the highest performance in terms of OER in 1 M KOH solution, which is related to the synergistic effect of multiple parameters including the optimal substitution amount of Co, the highest Brunauer−Emmett−Teller surface area, the smallest particle size among all samples (26.71 nm), and the lowest charge transfer resistance. The successful synthesis of ternary ferrites carried out for the first time via a microwave-assisted auto-combustion route opens up a new path for their applications in renewable energy technologies.