In the present study, the mechanical alloying process was used to produce the Ni-Nb-Si amorphous alloy. X-ray diffraction (XRD)analysis and high-resolution transmission electron microscopy (HRTEM) were used to approve the amorphous phase formation after 12 hours of mechanical alloying. The results obtained from the SEM morphological images of powder particles during mechanical alloying showed that increasing the milling time caused the reduction  of the powder particles size and uniformity in the shape of the particles. Enhancing the embrittlement and fracturing rate caused brittleness and the  increase in the  failure rate; these were followed by a decrease in the powder particle size to 1-5μm. Cold welding and flattening of the pure elemental powders after mechanical alloying for 2 hours formed a lamellar structure of the alternative layers of different elements lying over each other. SEM image of cross-section of powder particles showed that by increasing the milling time, the interlamellar spacing was decreased, the elements were distributed more uniformly, and finally, a uniform structure of theamorphous phase was completed.