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Developing non-noble metal-based electrocatalyst with high catalytic activity is essential for advancing hydrogen energy technologies. This study introduces a hydrothermal method for synthesizing order Ni(OH)2 nanosheets, with H3O40PW12 (denoted as PW12) loaded onto reduced graphene oxide (rGO) coated on nickel foam (referred to as PW12-Ni(OH)2/rGO). This method contrasts with the electrodeposition of Ni(OH)2, where PW12 is added to the synthetic system to direct the assembly and morphology of the Ni(OH)2 through a hydrothermal reaction. In this work, the nickel foam acts dual roles as both the substrate and the source of nickel for the formation of Ni(OH)2. The PW12-Ni(OH)2/rGO nanosheets, when successfully prepared and loaded onto the nickel foam (NF), exhibited superior electrocatalytic activity for the hydrogen evolution reaction (HER) in an alkaline electrolyte, achieving a current density of 10 mA·cm−² at an overpotential of 69 mV. Furthermore, we endeavored to expand the application of this material towards the oxygen evolution reaction (OER) by preparing PW12-(Fe/Co)Ni(OH)2/rGO through the addition of metal cations. This nanocomposite displayed outstanding electrocatalytic activity in alkaline electrolytes, with a current density of 10 mA·cm−² at an overpotential of 211 mV, and demonstrated excellent stability over a 50 h period in a 1 M KOH solution. The results presented in this paper offer an effective strategy for the preparation of polyoxometalate-based inorganic materials with diverse functionalities, applicable to both HER and OER.
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