Cu-Cr and Cu-Mo alloyed powders of different constitutes were investigated by X-ray diffraction (XRD) and TEM.Mo mainly dissovles in Cu lattice, and the solid solubility extension of Mo in Cu by mechanical alloying is limited. As Mo content increases, Cu grain size decreases, and the saturated amount of Mo in Cu increases. Amorphous phase appears in the Cu-80%Mo alloyed powder. Cu-Cr solid solution belongs to nano grain boudary solution. The alloyed product of Cu-50wt%Cr is affected by milling intensity. Cu nano crystallites and Cr oxides are formed with high milling intensity.