In this study, Cu-based Mo-doped composite powder was synthesized by ball milling technique. Elemental powder mixture containing 25 wt.% Mo was milled in a high-energy planetary-type ball mill to achieve homogeneously mixed composite powder. Characterization of the starting and the milled powders was carried out using scanning electron microscopy and laser diffraction analysis. It was found that particle size of powder had gradually decreased with increasing milling duration. scanning electron microscope pictures, corresponding to the later stages of milling process prove that nanocrystalline powders were obtained after milling duration of 30 h. Prolonged milling durations lead to powder contamination, which is undesirable for contact applications, where the purity is of big importance. Therefore, optimum milling duration was determined to be 30 h.