Electrodeposition of Ni, Cu and Ni-Cu alloys had been carried out in triethylammonium trifluoroacetate (TEATFA) medium on a glassy carbon (GC) electrode. Voltammetric investigations reveal that the reduction potential of Cu and the onset cathodic decomposition potential of Ni become close to each other favouring effective co-deposition of both these metals in TEATFA. Porosity and the surface roughness of the Ni-Cu alloys (obtained by constant potential electrolysis) considerably depend on the quantity of Cu, as confirmed by scanning electron microscopy (SEM) and atomic force microscopy (AFM). X-ray diffraction (XRD) reveals that the increase of Cu content in the Ni-Cu alloy leads to a decrease in the intensity ratio of I-(111)/I-(200) and a shift to low 2 theta value for Ni (1 1 1) plane. Potentiodynamic polarization and EIS analysis confirm that the Ni-Cu alloy containing more than 27% of Cu has low corrosion resistance. (C) 2014 Elsevier B.V. All rights reserved.