The Ni–Mo alloy coatings demonstrating high catalytic activity towards hydrogen evolution reaction were electrodeposited from a eutectic solvent composed of choline chloride and propylene glycol. The resulting alloys were characterized by spherical morphology and nanometric grain size (∼5–15 nm). XRD analysis indicated a gradient in phase composition with varying coating thickness, revealing that the coating surface was enriched with the Mo0.20Ni0.80 intermetallic compound. The obtained Ni–Mo alloy electrodes exhibited almost 3-times lower overpotential required to achieve a current density of 10 mA cm−2 compared to the reference Ni coating (−107 mV and −293 mV, respectively). The collected polarization and impedance data indicated that the enhancement in electrocatalytic activity was due to an increase in the real surface area of the alloy electrodes (Rf coefficient increased almost 9-times for Ni–Mo coatings compared to Ni coating). The electrocatalytic activity of the Ni–Mo alloy electrodes increased after successive CV cycles, attributed to changes in their surface composition (increase in current density by approx. 26% after 25 CV cycles).
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