In this paper the polarization characteristics of the processes of Ni and Co powders and Ni-Co alloy powders electrodeposition from ammonium sulfate containing supporting electrolyte are investigated as a function of Ni2+ and Co2+ ions concentrations. It is shown that the correct polarization curves for Ni and Co powders and Ni-Co alloy powders electrodeposition could be obtained only after IR drop correction, since the total current density of electrodeposition at the most negative potential of -1.4 V versus Ag vertical bar AgCl is extremely high (up to about 3-6 A cm(-2)) as a consequence of simultaneous hydrogen evolution which starts immediately after the beginning of metals (alloys) deposition. After determining the current density for hydrogen evolution and its subtraction from the total current density, correct polarization curves for Ni and Co powders and Ni-Co alloy powders electrodeposition are obtained. They are found to be different for each ratio of Ni2+/Co2+ ions concentration. It is also concluded that the shape of the polarization curves in all cases is practically defined by the shape of the polarization curve for hydrogen evolution. The morphology and composition of electrodeposited powders were also found to be sensitive to the ratio of Ni2+/Co2+ ions concentration. (c) 2006 Elsevier Ltd. All rights reserved.