Ni_(100-x)Mo_x(x=20, 30, 38) alloys have been synthesized by mechanical al-loying. The structure evolution of powders during mechanical alloying has been monitored byX-ray diffraction, SEM and TEM analysis. The Ni_(62)Mo_(38) sample becomes partially amor-phous after high energy ball milling, while the Ni_(80)Mo_(20) and Ni_(70)Mo_(30) become no-equilib-rium nano-crystals.