A crystalline Mg2Ni alloy has been prepared by mechanical alloying. Details of the ball milling conditions, such as milling time and milling speed of the equipment, have been investigated. Structure characterization, and the determination of particle distribution and surface properties of the alloyed powders were performed by using X-ray diffraction analysis, the Malvern particle analyser and scanning electron microscopy. It has been found that the crystalline alloy obtained by mechanical alloying has excellent surface properties compared with that prepared by a normal metallurgical method.