This work reports on the preparation of Ni-50Ti and Ni-40Ti-10Nb and Ni-30Ti- 20Nb (at.%) powders by high-energy ball milling and subsequent heat treatment. The milling process was carried out at room temperature in a planetary ball mill under Ar atmosphere. The as-milled powders were than heat-treated at 900oC for 1h under Ar atmosphere. X-ray diffraction (XRD), scanning electron microscopy (SEM), and microanalysis via energy dispersive spectroscopy (EDS) were used to characterize the milled and heat-treated powders. A metastable phase was initially formed in Ni-50Ti and Ni-40Ti-10Nb powders milled for 1h. Following the ball milling, the B2-NiTi compound was formed in these powder mixtures. The disordering of the B2-NiTi compound occurred owing the internal lattice strain after milling for 30h. Two phases were identified in Ni-50Ti and Ni-40Ti-10Nb powders milled for 60h: the metastable phase previously reported, and an amorphous phase. In Ni-30Ti-20Nb powders, it was noted the presence of an amorphous halo only. A structural relaxation of the B2-NiTi phase occurred in heat-treated Ni-50Ti, Ni-40Ti-10Nb, and Ni-30Ti-20Nb powders. A small amount of Ni3Ti and NiTi2 was also formed after heat treatment at 900oC for 1h, and an iron contamination lower than 2at.% was found.