In this report, a nickel nanoscaled morphology was synthesized by two-step cathodic electrodeposition on a microporous copper template. The resulting morphology, nanosheets formed on 3D micropores, offers incredible cyclic stability of almost 100% and facilitates transport mechanisms while significantly preserving the active surface area. The origin of the nanosheets is assumed to be the presence of a small amount of iron cations in the electrolyte bath during the final deposition step. By altering the deposition current density of this step, three samples were prepared and compared in terms of the resulting morphology, chemical composition, surface area, wettability, and activation toward the methanol oxidation Reaction. Results show that an increase in the deposition current density in the range of this study produces finer and denser nanosheets, a higher content of reduced iron, a larger surface area, and greater activity toward MOR. The current density for methanol oxidation was exceptional among all other studies on nickel-containing electrocatalysts, yielding a steady-state current density of 135 mA cm–2 at 600 mV versus SCE. All samples offered superhydrophilicity.

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