Besides reducing pollution and removing urea from wastewater, electro-oxidation of urea has also offered new prospects for filling the overall water gap for economically producing hydrogen. In this regard, a simple and low-cost electrochemical deposition technique was used to prepare a highly efficient bifunctional electrocatalyst for HER and UOR (in place of OER) on nickel foam (NiFeSP/NF). The three-dimensional and nanoporous NiFeSP/NF electrocatalyst demonstrated relatively high stability and electrocatalytic activity. Notably, the bimetallic and dual-anionic NiFeSP/NF electrode demonstrated good performance for HER (33, 105, and 132 mV at current densities of -10, -100, and -200 mA.cm-2, correspondingly), OER (1.451, 1.502, 1.528, 1.576 V vs. RHE at 10, 100, 200 and 400 mA.cm-2), and UOR (1.304, 1.346, 1.389 and 1.473 V vs. RHE at current densities of 10, 100, 200 and 400 mA.cm-2, in turn). Moreover, the use of the NiFeSP/NF||NiFeSP/NF pair as anode and cathode in an overall water-splitting system assisted by urea achieved 1.348 and 1.582 V vs. RHE at 10 and 100 mA.cm-2 in 1000.0 mM KOH with 330.0 mM urea solution, which is 163 and 234 mV lower than those conducted in 1000.0 mM KOH alkaline solution, respectively. Additionally, the NiFeSP/NF||NiFeSP/NF pair demonstrates long-term stability (30 h) in the chronopotentiometry test at 100 mA.cm-2 in 1000.0 mM KOH with 330.0 mM urea solution. This bimetallic and dual-anionic NiFeSP electrode exhibits substantial catalytic activity due to the appropriate synergy, between Fe and Ni, the modification of electronic structure enabled by the dual-anionic, and the enhanced electrocatalytic active surface caused by high porosity. The low cost and single-step manufacturing method of the NiFeSP electrode, high electrocatalytic activity, and stability make it potentially ideal for commercial use in hydrogen generation and wastewater treatment containing urea

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