Abstract: Nanocrystalline powders in the Ni-Ti and Ni-Cr systems were prepared by mechanical alloying (MA) of elemental crystalline powders in an inert atmosphere. The microstructure of the mechanically alloyed powders were characterized by XRD and TEM. The ball-milling process results in a drastic decrease of the crystallite size to the nanometer scale. X-ray diffraction analysis reveals that in the Ni-Cr system, no diffraction peaks from NiCr compound were observed even after 20 h of ball milling; while the lattice parameter of Ni increased with the milling time. In the Ni-Ti system, amorphous alloy was formed. Crystalline intermetallic compounds were obtained by post heat treatment of the amorphous alloy.The crystallization temperature of the amorphous NiTi alloy was obtained be DSC measurement.