Multilayer nickel–copper coatings consisting of layers of nickel–copper alloy and a mixture of metals with hydroxides were obtained by electrodeposition from polyligand pyrophosphate–ammonia electrolyte by the two-pulse potentiostatic method. A comparison between two different electrodes with the same real surface area is presented. The equality of the surface area of electrodes deposited from the electrolyte containing different copper and nickel ions’ concentration ratio was achieved by deposition of different numbers of layers. It is shown that the increase in the copper content in electrolyte leads to an increase in the copper ions’ content in the coating and the electrode surface develops more intensively. Freshly deposited coatings have approximately the same catalytic activity in the glucose oxidation reaction in the alkaline solution. But a multilayer coating with a higher copper content is more corrosion resistant and more stable in long-term electrolysis.

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