Nanocrystalline Ni (50−X) Ti 50 Cu X (X = 5, 9 wt%) alloys were successfully produced by mechanical alloying. Mechanical activation was performed at different milling times under a high purity argon (99.998 vol%) atmosphere. Phase analysis and structural features of the samples were examined by X-ray diffraction (XRD). Results revealed that NiTiCu (B2) phase was achieved after 600 min of milling. The formation of this phase was mostly related to the critical factors in determining the site replacement of elements in Ni-Ti-Cu ternary system. After 600 min of milling, the average crystallite size and lattice strain of the samples were about 5 -10 nm and 1.057% -1.967%, respectively. Evaluation of the full width at half maximum (FWHM) values for all the samples indicated the occurrence of anisotropic line broadening. The determined amounts of crystallinity revealed that the fraction of crystalline phase decreased with increasing weight percentage of copper up to 9% and reached a minimum value after 600 min of milling. The lattice parameters and the unit cell volume of the milled samples were always larger than the standard values. In addition, lattice parameter deviation influenced by the weight percentage of copper. Based on the obtained data, mechanical alloying process can be used for production of nanocrystalline NiTiCu alloys with different structural features.