<p>Electrodeposition activation of metal–organic frameworks (MOFs) has emerged as a promising strategy for the synthesis of highly efficient electrocatalysts for oxygen evolution reaction (OER). Herein, a cathodic electrodeposition method is presented to activate NiFe-based MOF nanosheets on a nickel foam (NF) support to form a NiFe-MOF/(oxy)hydroxide nanocomposite (A-NiFe-TDC). This activation route not only creates abundant defective structures but also involves partial valency reduction in Ni/Fe species and electron transfer to grow a new component of NiFe-(oxy)hydroxide on the surface of the NiFe-TDC MOF. By adjusting electrodeposition times and Ni/Fe mol ratios, the as-prepared A-NiFe-TDC-5 nanocomposite exhibits improved electrocatalytic performance for OER in an alkaline medium, achieving a high current density of 100&#xa0;mA&#xa0;cm⁻² at a low overpotential of 242.9&#xa0;mV, a small Tafel slope of 24.9&#xa0;mV dec⁻¹, and good long-term stability over 450&#xa0;h. After OER, A-NiFe-TDC-5 is self-reconstructed to form NiFe-OOH nanosheets, contributing to optimizing the electronic structures and further improving the electrocatalytic activity and stability. This work provides a viable and effective electrodeposition activation method for the preparation of MOF-based nanocomposites to boost the electrocatalytic performance for OER.</p> Graphical abstract <p></p>