Electrodeposition of Copper–Nickel Foams: From Separate Phases to Solid Solution

Copper-based electrocatalytic materials with high surface area are essential for various processes, such as water splitting and the electroreduction of carbon dioxide and nitrates. Three-dimensional nanostructured electrodes offer distinct advantages in these applications due to their expansive surface area, which enhances charge transfer and mass transport. For bimetallic systems, however, the phase state, whether a solid solution or a mechanical mixture of metals, is critically important for catalytic performance. This study explores the formation of Cu-Ni solid solutions via electrodeposition using the dynamic hydrogen bubble template method. Two types of electrolyte were employed: sulfate-based and citrate-based. Through characterization by X-ray diffraction, scanning electron microscopy, elemental mapping, and X-ray fluorescence spectroscopy, we demonstrate that metallic foams deposited from sulfate solutions are heterogeneous, with poor control over nickel content. In contrast, the use of citrate-based solutions allows the nickel content in the deposits to be effectively controlled by varying the solution composition, thereby enabling the formation of a solid solution.