Preparation of high surface area Cu‐Au bimetallic nanostructured materials by co‐electrodeposition in a deep eutectic solvent

•Co-electrodeposition of Cu and Au bimetallic films has been conducted in a deep eutectic solvent.•Bimetallic Cu and Au nanostructures with variable morphology and composition are obtained.•Lead underpotential deposition on Cu-Au films has been used to assess the electroactive surface area.•Cu-Au films had an electroactive surface area five to 14 times higher than the geometric area. Our sustainable future requires finding new, affordable and green routes to prepare nanostructured materials used in renewable energy conversion. In this work we present an electrodeposition method in a deep eutectic solvent (DES) to prepare bimetallic high surface area nanostructures of Cu and Au with tunable structure and composition. The metal electrodeposition performed in choline chloride within a urea deep eutectic solvent allows us to tailor the size, morphology and elemental composition of the deposits. We combine electrochemical methods with scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and energy dispersive X-ray spectroscopy (EDS) to characterize the electrodeposited nanostructured materials. We assess the increase of the electroactive surface area through the analysis of the lead underpotential deposition (UPD) on the prepared films. Integrated Pb UPD charge values of ca. 1600–4000 μC/cm2 for the prepared Cu-Au films have been calculated, suggesting a 5–14 fold increase of the active surface area compared to flat surfaces of polycrystalline Cu or Au. Our work reports a versatile and environmentally friendly route for the electrodeposition of Cu-Au bimetallic nanostructures in a DES. The combination of a tailored morphology and composition with the high active surface area of the nanostructured materials show that electrodeposition in DES is promising for the development of multimetallic electrocatalysts. [Display omitted] .