NiAl alloy powders were prepared by mechanical alloying method and bulk specimens were produced using hot isostatic pressing techniques. This study focused on the transformation behavior and properties of Ni-Al mechanically alloyed powders and bulk alloys. Transformation behavior was investigated by differential scanning calorimeter (DSC), XRD and TEM. Particle size distribution and microstructures of mechanically alloyed powders were studied by particle size analyzer and scanning electron microscope (SEM). After 10 hours milling, XRB peak broadening appeared at the alloyed powders with compositions of Ni-36at%Al to 40at%Al. The NiAl and intermetallic compounds were formed after water quenching of solution treated powders and bulk samples at , but the martensite phase was observed after liquid nitrogen quenching of solution treated powders. However, the formation of intermetallic compounds were not restricted by fast quenching into liquid nitrogen. It is considered to be caused by fast diffusion of atoms for the formation of stable (NiAl) phase and due to nano sized grains during quenching. Amounts of martensite phase increased as the composition of aluminium component decreased in the Ni-Al alloy, which resulted in the increasing damping properties.