This paper presents results on the synthesis of Cu-Pd alloy thin films on Ti substrates by co-electrodeposition of Pd and Cu from nitrate-base electrolytic baths. The deposition rates of Cu and Pd were determined by Electrochemical Quartz Crystal Microbalance as a function of the electrode potential and Cu+2 and Pd+2 concentrations. It is shown that electrodeposition of copper and palladium occurs simultaneously at -0.50V vs. SCE and that Cu-Pd thin films over the entire composition range were obtained by changing the composition of the solution. X-ray diffraction analyses indicated that these films have a nanocrystalline single-phase face-centered cubic structure and scanning electron microscopy analyses showed that potentiostatically deposited films are rough and porous, which is appropriate for electrocatalysis applications. In an attempt to get denser deposits as required for H-2 purification applications, pulsed potential co-electrodeposition was performed and the effect of the deposition conditions on the roughness of the films was assessed by double layer capacitance measurements. It was shown that smooth Cu-Pd films (with R-f value as low as 8, as opposed to more than 120 for films prepared in the potentiostatic mode) could be obtained with a proper choice on the deposition conditions. (C) 2011 Elsevier Ltd. All rights reserved.