α-Ni(OH)2 exhibits a higher intrinsic UOR catalytic activity and durable stability in comparison with its nickel hydroxide counterpart β-Ni(OH)2.

Urea oxidation reaction (UOR) has received a high level of recent interest since electrochemical oxidation of urea can remediate harmful nitrogen compounds in wastewater and accomplish hydrogen fuel production simultaneously. Thus, urea is considered to be potential hydrogen energy source that is inherently safe for fuel cell applications. However, the catalytic reaction suffers from slow kinetics due to six electron transfer in UOR. In this work, β phase NiS is successfully prepared through facile hydrothermal reaction, in which diethanolamine (DEA) was added as chelating agent leading to 3D nanoflower morphology. The crystal structure, surface morphology, and chemical bonding of the β−NiS were characterized by X–ray diffraction (XRD), scanning electron microscope (SEM), and X−ray photoelectron spectroscopy (XPS), respectively. The UOR performance of NiS was evaluated by means of linear sweep voltammetry (LSV), Tafel analysis, electrochemical impedance spectroscopy (EIS), chronoamperometry, and chronopotentiometry in 1 M KOH electrolyte containing 0.33 M urea. Compared to the Ni(OH)2 counterpart, NiS exhibits lower onset potential, increased current responses, faster kinetics of urea oxidation, lower charge transfer resistance, and higher urea diffusion coefficient, leading to the enhanced catalytic performance toward UOR. Moreover, the developed NiS catalyst exhibits superior stability and tolerance towards urea electro−oxidation in 10,000 s test.

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