Development of a cost-effective and efficient electrocatalyst for the sluggish oxygen reduction reaction (ORR) is a crucial challenge for clean energy technologies. In this study, we have synthesized various Ni and Co oxide (NCO) nanomaterials via a facile coprecipitation, followed by the calcination method. The morphology of the formed NCO nanomaterials was controlled by varying the percentage of the Ni and Co precursors, leading to the formation of a template-free mesoporous spinel phase structure of Ni xCo3- xO4. It was found that the number of the octahedral site cations and the defect sites with lower oxygen in the spinel oxides can be tunable by taking appropriate ratios of the Ni and Co precursors. The optimized NCO nanomaterial exhibits superior electrocatalytic activity compared to the mono-metal oxides of NiO and Co3O4 with over 3 times higher current density and ∼0.250 V lower onset potential toward ORR in a 0.1 M KOH solution. Scanning electrochemical microscopy was utilized in mapping the activity of the catalyst and monitoring the ORR products, further confirming that a four-electron transfer pathway was facilitated by the NCO nanomaterial. Moreover, the developed mesoporous NCO nanomaterial exhibits a high methanol tolerance capability and long-term stability when compared to the commercial state-of-the-art Pt/C electrocatalyst. The improvement of the catalytic activity and stability of this advanced NCO nanomaterial toward ORR may be attributed to the facile accessible mesoporous structure, and the abundance of octahedral site cations and defective oxygen sites.
Keywords: SECM; mesoporous; nanomaterials; nickel-cobalt oxide; oxygen reduction.