Mg60Zn35Ca5 amorphous powder alloys were synthesized by mechanical alloying (MA) technique. The results of the influence of high-energy ball-milling time on amorphization of the Mg60Zn35Ca5 elemental blend (intended for biomedical application) were presented in the study. The amorphization process was investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM). Initial elemental powders were mechanically alloyed in a Spex 8000 high-energy ball mill at different milling times (from 3 to 24 h). Observation of the powder morphology after various stages of milling leads to the conclusion that with the increase of the milling time the size of the powder particles as well as the degree of aggregation change. The partially amorphous powders were obtained in the Mg60Zn35Ca5 alloy after milling for 13-18h. The results indicate that this technique is a powerful process for preparing Mg60Zn35Ca5 alloys with amorphous and nanocrystalline structure.