A Study of Cu‐Rh Electrodeposition**

This manuscript reports the simultaneous electrodeposition of Cu and Rh from an aqueous nitrate solution. The early stages nucleation growth bimetallic layer were explored using techniques such as cyclic voltammetry current transients. Non-dimensional Scharifker-Hills graphs showed occurrence diffusion-controlled three-dimensional best described by Volmer-Weber mechanism. Additionally, different ratios Cu−Rh electrodes synthesized varying potential deposition content in bath. Characterization including electron microscopy, x-ray diffraction, photoelectron spectroscopy employed to investigate chemical composition structure deposits. results a higher amount Cu2+ species than Cu+/Cu0 when more negative was applied, present high amounts final morphology obtained material proved be dependent on potentials : content, showing interdependency between metals.