Fe, Si and B powders, mixed with atomic composition Fe78Si9B13, are subjected after arc melting to a melt spinning process, which is optimized to obtain the greatest amount of amorphous ribbon. The amorphous ribbons are milled to powder form in a vibratory ball mill and a vibratory disc mill, taking care of maintaining the amorphous character. Ribbons and powders have been characterized by X-ray diffraction (XRD), laser diffraction, SEM and TEM microscopy, and differential scanning calorimetry (DSC). The amorphous character and particle size of the powders are characterized as a function of the mill charge and the milling time. It is shown that the use of the ball mill is appropriate for obtaining small quantities of amorphous or nanocrystalline powder, while the disc mill can process larger quantities of powder in a shorter time. The particle sizes obtained for milling times between 10 and 150 min range between 26 and 412 μm, ready for use in powder metallurgy processes.