A wide compositional range of Ni-Pd alloy catalysts were prepared by electrodeposition for use as anode materials for methanol oxidative fuel cells in alkaline conditions. Structural characterization of the electrocatalysts in their as-plated condition revealed that the Ni-Pd catalysts synthesized were nanocrystalline, single phase, face centered cubic materials, indicating the formation of complete solid solution in the alloy. Compositional analysis of the alloys indicated that the palladium composition of the alloy increased with decrease in current density. This change in the composition of the alloy resulted in a shift in the X-ray diffraction peaks. The percentage shift in the d-spacing calculated from X-ray diffraction is in good agreement with percentage of palladium in the alloy. The electrocatalysts prepared are active for methanol oxidation in alkaline medium. © 2007 Elsevier B.V. All rights reserved.