The exploration of earth-abundant catalysts that are highly active and robustly stable for urea electrooxidation is critical for energy-efficient hydrogen production associated with urea-rich wastewater purification. Herein, Co-doped α-Ni(OH)₂ hybrid films with unique ultrafine nanoparticles assembled network structure are constructed as efficient bifunctional electrocatalysts for urea-assisted water electrolysis. By employing a facile potentiodynamic deposition route carried out in a deep eutectic solvent (Ethaline), ultrafine Ni-based nanoparticles with a α-Ni(OH)₂ rich surface doping by Co are in-situ grown on Cu foam substrate (Co_x-Ni(OH)₂ NPs/CF), creating an integrated electrode full of intimate contact interfaces. The doping of Co triggers a structural transition with electronic structure changes at the electrode surface and lowers the onset potential required for Ni(OH)₂/NiOOH, which strongly enhances the urea electrolysis activity. Through potential conditioning procedure, the optimized Co_0.26-Ni(OH)₂ NPs/CF catalyst (with a Ni/Co proportion of 1:0.26) manifests excellent electrocatalytic performance for urea electrolysis in 1.0 M KOH with 0.5 M urea, presenting a low onset potential of 1.27 V vs. RHE for urea oxidation and an overpotential of 106 mV for the hydrogen evolution reaction at 10 mA cm⁻². Impressively, the constructed alkaline urea electrolyzer based on Co_0.26-Ni(OH)₂ NPs/CF delivers 10 mA cm⁻² at a stable output voltage of 1.42 V with robust durability over 38 h and high selectivity.

探索对尿素电氧化具有高活性和稳健性的富土催化剂，对于与富尿素废水净化相关的高能效氢气生产至关重要。在本文中，具有独特的超细纳米颗粒组装网络结构的共掺杂α-Ni（OH）₂杂化膜被构建为用于尿素辅助水电解的高效双功能电催化剂。通过使用在低共熔溶剂（Ethaline）中进行的简便的电势沉积路径，在Cu泡沫基材（Co _x-上原位生长具有Co富集α-Ni（OH）_2的超细Ni基纳米颗粒。镍（OH）₂NPs / CF），创建一个充满紧密接触界面的集成电极。Co的掺杂触发了电极表面电子结构变化的结构转变，并降低了Ni（OH）₂ / NiOOH所需的起始电势，从而极大地增强了尿素的电解活性。通过电位调节程序，优化的Co _0.26- Ni（OH）₂ NPs / CF催化剂（Ni / Co比例为1：0.26）在1.0 M KOH和0.5 M尿素中表现出优异的电催化尿素电催化性能，显示出较低的尿素氧化的RHE起始电位为1.27 V vs. RHE，10 mA cm ^-2时氢气释放反应的过电位为106 mV。令人印象深刻的是，基于Co _0.26- Ni（OH）₂ NPs / CF的碱性尿素电解槽在 1.42 V的稳定输出电压下可提供10 mA cm ^-2的电压，在38小时内具有出色的耐用性和高选择性。