Co-Ni nanowires arrays were obtained by electrochemical template synthesis in a polycarbonate track etched (PCTE) membrane. To diminish the effects of anomalous deposition observed in the Co-Ni system, the electrochemical deposition was performed from a solution containing nickel and cobalt in an atomic ratio of 3:1. Electrochemical deposition was performed at constant potentials E = -0.8, -0.9, -1.0, -1.1, -1.2 V vs Ag/AgCl for 15 min. The structures were characterized electrochemically via cyclic voltammetry, chronoamperometry, and charge stripping. Co-Ni nanowires were characterized by scanning electron microscopy (SEM/EDAX) to assess the morphology and the composition of the Co-Ni alloy nanowires at different deposition potentials. Electrochemical and structural analysis provided details of their deposition kinetics, structure, and morphology, which would be used to build nanowires array with controlled structure and composition.