Fe, Si, B, Cu, Nb powders with an atomic ratio of Fe73.5Si13.5B9Cu1Nb3, are subjected to an electric arc melting process and subsequent amorphisation by melt spinning after compaction. The amorphisation process is optimised to obtain the highest amount of amorphous ribbon according to the critical processing parameters. The amorphous ribbons are milled to powder in a vibratory disc mill by adjusting the milling parameters in order to preserve the amorphous character. The ribbons and powders have been characterised by X-ray diffraction (XRD), laser diffraction and SEM and TEM microscopy. The amorphous character and particle size of the powders are characterised as a function of milling time. The particle sizes obtained for milling times between 30 and 120 min range between 123 and 69 µm, ready for use in PM processes.