In this paper, the high performance Cu-Fe-P alloys with ultra-fine grain and nanocrystalline structure were successfully prepared by mechanical alloying (MA) and reactive hot-pressing (RHP). Then the combined effects of sintering temperature and phosphorus content on microstructure and properties were investigated. The results showed that phosphorus had a positive effect on the performance of Cu-Fe-P alloy. It could reduce the content of iron doped in the Cu matrix rather than forming precipitates such as Fe3P or Fe2P. Moreover, the ultra-fine grain and nanocrystalline structure had a great effect on performance of the alloys. The crystallite size of the Cu-Fe-P alloys exhibited average value of 10 nm after milling for 4 h by TEM. The lower sintering temperature was better to retain the size of nanoparticles and achieve excellent performance. Consequently, the best performance was achieved by the Cu-Fe-0.025P sintered at 600 degrees C and ball-milled for 4 h. The electrical conductivity reached 80.41% IACS with the tensile strength of 517 MPa which was much better than the conventional Cu-Fe-P alloy.