Nanocrystalline Ni 50 Al 50− Mo ( = 0, 0.5, 1, 2.5, 5) intermetallic compound was produced through mechanical alloying of nickel, aluminum, and molybdenum powders. Powders produced from milling were analyzed using scanning electron microscopy (SEM) and X-ray diffractometry (XRD). Results showed that, with increasing the atomic percent of molybdenum, average grain size decreased from 3 to 0.5 m. Parameter lattice and lattice strain increased with increasing the atomic percent of molybdenum, while the crystal structure became finer up to 10 nm. Also, maximum microhardness was obtained for NiAl 49 Mo 1 alloy.