By means of surface mechanical attrition treatment (SMAT), a nanocrystalline (NC) surface layer was obtained on Cu-10Ni Alloy. The electrochemical corrosion behavior of three samples, i.e. the original coarse grain ones, the SMAT for 60 min ones, and the ones SMAT for 60 min plus annealed at 200℃ for 6 h, was investigated by means of potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) techniques in 0.05 mol/ L Na2SO4 + 0.05 mol/L H2 SO4 solution. The result showed that the corrosion potential of the SMAT Cu-10Ni Alloy shifted to a more negative value with respect to the un-treated alloy claerly Implying a decrease of the corrosion resistance of Cu-10Ni alloy after SMAT. However, the SMAT alloy exhibited passivation behavior to certain extent in its polarization curve.