In‐Situ Electrodeposition Self‐Supported Bimetallic Sulfides for Urea Electrooxidation

The electrocatalytic urea oxidation reaction (UOR) is considered an effective pathway for hydrogen generation due to its lower theoretical potential, replacing the traditional oxygen evolution reaction (OER). However, the UOR requires the development of high‐performance and stable catalysts to overcome this slow kinetics challenge. Herein, we successfully prepared self‐supported bimetallic sulfides (NiCoS) with a layered nanosheet structure on carbon paper (CP) via a one‐step electrodeposition method. The morphology and phase composition of the NiCoS/CP were characterized. Electrochemical tests revealed that the NiCoS/CP electrode achieved 10 mA cm‐2 at 1.46 V (vs. RHE) in an alkaline urea solution and exhibited a Tafel slope of 48.02 mV dec‐1. Additionally, a two‐electrode system was constructed using NiCoS/CP as the anode and a platinum plate as the cathode. In this system, the urea electrolysis process operated at a voltage of just 1.6 V to achieve a current density of 10 mA cm‐2. This voltage is 130 mV lower than what is typically required for traditional water electrolysis, highlighting substantial energy savings. The high activity of the NiCoS/CP electrode is attributed to its self‐supported design, layered nanosheet structure, and the synergistic effects between Ni and Co, making it a highly promising catalyst for urea oxidation.