Starting from arc-melted alloys, nanostructured Pr 0.5 Sm 0.5 Co 5 powders were synthesized by mechanical milling and subsequent vacuum annealing during short times to develop an optimal microstructure with high hard magnetic properties. The best magnetic properties were obtained for the stoichiometric Pr 0.5 Sm 0.5 Co 5 powders milled for 4h and annealed at 800°C for 1min with a high coercitivity of 13.5kOe, a high M r /M max ratio of 0.72 and a maximum energy product of 11MGOe. From X-ray diffraction and transmission electron microscopy, CaCu 5 -type phase and an average grain size of about 12nm were determined in the annealed powders, and we calculated that 59% of the volume of the grains/crystallites are exchange-coupled. The observed magnetic hardening is associated to the high magnetic anisotropy field of the PrCo 5 and SmCo 5 phases and also to the microstructure developed by the processing used.