Nanocast Mixed Ni–Co–Mn Oxides with Controlled Surface and Pore Structure for Electrochemical Oxygen Evolution Reaction

Nanocasting or hard-templating is a versatile method to produce ordered mesoporous mixed transition metal oxides (MTMOs) with promising potential for both oxygen evolution reaction (OER) and oxygen reduction reaction (ORR). Herein, a comprehensive investigation was conducted on various Ni_xCo_yMn_zO₄ replicated from large pore KIT-6 silica. The materials were calcined at different temperatures to study the influence of the oxide formation and the resulting pore structure ordering, as well as surface properties, on the electrochemical activity and stability of the catalysts. After a comprehensive characterization, electrocatalytic performances of the materials were investigated in detail for OER to find a structure–activity relationship. In OER, a correlation was established between calcination temperature, pore and surface properties, and the overall efficiency and stability. The best sample, Ni_xCo_yMn_zO₄ calcined at 300 °C, provided a reasonable current density (25 mA/cm² at 1.7 V vs RHE) and an overpotential of 400 mV at 10 mA/cm², and demonstrated increased current density (above 200 mA/cm² at 1.7 V vs RHE) once loaded into a Ni foam compared to the bare foam. This sample also remained stable over 15 h. Our results indicate that the calcination temperature greatly affects the porosity, crystalline structure, phase composition, and the activity of the catalysts toward OER.