Ni Surface & Polyacryloyl Hydrazide Mediated Growth of Co₃O₄@NiCu Alloy Nanocuboids for Effective Methanol Oxidation and Oxygen Evolution Reactions

Abstract Strategies to control the size, shape, and lattice arrangement, introduce doping agents, and induce heterostructuring in electrocatalysts are strongly desirable to tailor their activities. Herewith, a one‐pot strategy utilizing polyacryloyl hydrazide (PAHz) as the composition directing agent and metallic Ni surface as the shape directing agent is employed to grow Co₃O₄ doped NiCu alloy nanocuboids on Ni foam (NF) under hydrothermal conditions for electrocatalytic H₂ production. The resulting bi‐functional electrodes are suitable for methanol oxidation reaction (MOR) coupled green H₂ production with effective energy efficiency. The low overall potential (MOR+HER) of 1.78 V to realize the current density (j) value of 100 mA cm⁻² and extended durability (100 h@10 mA cm⁻²) along with the selective conversion of methanol to formate support the viability of the NF‐PAHz‐Co₃O₄@NiCu for the said operation. The electrode also displays efficacy toward oxygen evolution reaction (OER) activity and j_OER value of 100 mA cm⁻² is realized at a potential value of 1.65 V_RHE with adequate durability. Overall, the synthetic strategy is general, scalable and may be extended to grow other metal oxide doped alloy nanostructures in the future.