<p>Water electrolysis is a crucial technology for renewable energy conversion and storage, yet its progress is hindered by high overpotentials. The development of cost-effective, stable, non-precious metal catalysts with high activity is essential. In this study, a 3D flower-like NiCo-layered double hydroxide (LDH) structure is synthesized via a hydrothermal method, followed by Fe³⁺ doping through FeCl₃6H₂O etching to produce Fe-doped NiCo-LDH (NCF-LDH). Under alkaline conditions, the NCF-LDH electrode demonstrates remarkable electrocatalytic performance for the oxygen evolution reaction (OER), attaining low overpotential of 263 mV at the current density of 50&#xa0;mA cm^− 2 and a Tafel slope of 71.9 mV dec^− 1, accompanied by exceptional operational stability. The enhanced catalytic performance results from the synergistic effects of the 3D flower-like architecture, which provides a large specific surface area, exposing abundant active sites and promoting efficient charge transfer. Additionally, the Fe³⁺ induced lattice distortion and generation of vacancies disrupt the atomic arrangement, creating defect-rich sites that enhance OER activity.</p>