Morphology-Driven Enhancement of Alkaline OER Performance in Spinel NiCo₂O₄ Nanosheet Electrodes

The oxygen evolution reaction (OER) is a critical anodic process in alkaline water electrolysis, and its catalytic performance can be effectively regulated through rational morphology engineering that governs active-site exposure, mass transport, and charge-transfer kinetics. Herein, we report a precursor-controlled synthesis of spinel NiCo₂O₄ (NCO) catalysts with tunable two-dimensional architectures for efficient alkaline OER. By employing hexamethylenetetramine (H) and urea (U) as precipitating agents, the NiCo₂O₄ catalysts with distinctly different nanosheet morphologies were directly grown on nickel foam. The NCO-H catalyst exhibits substantially enhanced OER activity by achieving lower overpotential of 259 mV, a smaller Tafel slope of 84 mV dec^–1, and higher turnover frequency compared to NCO-U catalyst. The superior OER performance is attributed to an ultrathin, highly interconnected nanosheet network that provides abundant accessible active sites, shortened ion-diffusion pathways, and accelerated interfacial charge transfer. Moreover, the optimized electrode demonstrates excellent durability (50 h) with negligible potential degradation after the partial surface transformation into an oxyhydroxide-rich active phase, while post-stability polarization and impedance analyses confirm the preservation of catalytic integrity. These findings highlight precursor-regulated morphology engineering as an effective strategy for optimizing the electrocatalytic performance of spinel oxides and establish NiCo₂O₄ as a robust, earth-abundant OER catalyst for alkaline water-splitting applications.