The synergistic effects of doping and interface engineering enhance the oxygen evolution reaction catalysis of Ni3Se2–Mo@NiFe-LDH

Highly efficient, cost-effective, and durable electrocatalysts are crucial for scalable renewable hydrogen production via water electrolysis. Herein, a Ni 3 Se 2 –Mo@NiFe-LDH composite catalyst was synthesized through a hierarchical strategy combining two-step hydrothermal treatment and electrodeposition. The catalyst exhibits outstanding OER performance, delivering a low overpotential of 205 mV at 10 mA cm −2 and stable operation for 200 h. In this heterostructure, the conductive Ni 3 Se 2 core promotes electron transport, while the in-situ formed NiMoO 4 phase regulates the electronic structure to optimize oxygen intermediate adsorption. Meanwhile, the NiFe-LDH shell undergoes surface reconstruction during operation, forming an active oxyhydroxide layer that activates the lattice oxygen mechanism (LOM). Operando Raman spectroscopy and post-stability analyses (XPS, SEM, ICP-OES) verify the formation of the active phase and preserved structural integrity. The synergistic effects of electronic modulation and interfacial engineering accelerate charge transfer and reduce OER kinetic barriers, offering an effective strategy for developing high-performance non-precious-metal OER catalysts.