Nanocrystalline Ag-28Cu supersaturated solid solution is prepared by mechanical alloying (MA) using a planetary ball mill. The mechanical alloyed powders are characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM) and differential scanning calorimeter (DSC). XRD patterns show that the main peak of Ag-28Cu supersaturated solid solution exists at about 2θ=39° when the milling time is 30h. HRTEM images show that the grain sizes of as-prepared solid solutions have distributions from 10nm to 15nm. The interplanar spacing of (111) plane for fcc Ag-28Cu supersaturated solid solution is about 2.24Å. DSC measurement result indicates that the melting temperature of Ag-28Cu supersaturated solid solution is 783.8°C. The Ag(Cu) supersaturated solid solutions are in metastable state and they will be transformed into Ag-rich phase and Cu-rich phase simultaneously by annealing at 215°C- 415°C.