Copper alloys with different amounts of zinc were synthesized via high energy ball milling at liquid nitrogen and room temperature. Bulk samples were produced in situ by controlling the milling temperature. It is shown that temperature plays an important role in formation of artifact-free consolidated samples via its effect on defect formation and annihilation during the milling process. The mechanical behavior of Cu-Zn nanocrystalline alloys was examined using Vickers microhardness and tensile tests. The nanostructure of the alloys was investigated by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The hardness results of processed alloys vary as a function of the alloying elements. Considering typical low ductility of nanocrystalline materials, the improved ductility with the high strength observed in these alloys suggests that they are artifact-free and may have several deformation mechanisms, which may include dislocation activity and nano-twinning.