The nickel-bismuth binary coatings with various chemical compositions were galvanostatically deposited on the copper electrode in view of their possible applications as electrocatalytic materials for the hydrogen evolution reaction (HER) in alkaline solution. The HER activity of coatings was tested with the help of potentiodynamic measurements and electrochemical impedance spectroscopy (EIS) technique. The electrochemical characterization was achieved by the means of cyclic voltammetry (CV). The surface morphology and surface composition of coatings were determined with scanning electron microscopy (SEM), and energy dispersive X-ray (EDX). The potentiodynamic measurements show that, the binary coatings decrease the hydrogen over potential and increase the current density values for HER. The EIS analysis confirms, the charge transfer resistances decrease and the double layer capacitance values increase for binary coatings. The EDX results in sign that the composition of binary coating changes by using coating bath. The Cu/NiBi-2 coating (Ni2+/Bi3+ is 99.71:0.29 molar ratio) is the best suitable cathode composition for the HER in alkaline media under these experimental conditions. (C) 2011 Elsevier B. V. All rights reserved.