A new electrolytic bath containing sodium perchlorate, thiourea, sodium gluconate, boric acid and silver and cobalt salts, able to favour simultaneous electrodeposition of silver and cobalt, has been developed. A systematic analysis of the effect of cobalt(II) concentration, applied deposition potential, hydrodynamic conditions and electrochemical techniques was made. From this bath, Co-Ag deposits of different composition have been prepared and characterized. Granular deposits were obtained from all the electrochemical deposition procedures tested; more compactness and uniformity were attained when the deposits were obtained by pulse plating method. Electrochemical and compositional characterizations indicated that heterogeneous cobalt-silver deposits were prepared containing some oxi- and/or hydroxylated cobalt species. (C) 2008 Elsevier B.V. All rights reserved.