A comparison was performed between Co-Ni thin films and template-assisted nanowires arrays obtained by electrochemical co-deposition. To reduce the effects of anomalous deposition and increase the Ni content in the deposit, an electrolyte with three times more Ni than Co in atomic ratio was chosen. Electrochemical deposition was performed at constant potentials chosen in the range from E = −0.8 to −1.2 V vs. Ag/AgCl. Cyclic voltammetry, chronoamperometry, and charge stripping techniques were used to characterize and compare the electrochemical behavior of Co-Ni films and nanowires. Morphological and compositional characterization was performed by scanning electron microscopy (SEM/EDAX) to assess the influence of the deposition potential on the growth of film and nanowires. A comprehensive analysis of the deposit growth rates for thin films and nanowires is presented taking into consideration the hydrogen evolution and anomalous deposition. The comparative study of the composition of film and nanowires obtained at different deposition potentials has shown that deposition of nanowires with a film-like composition takes place at more positive potential than thin film.
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