Cu 54 Hf 36 Al 10 amorphous/nanocrystalline composite particles were prepared by ball-milling. Crystalline master alloys were prepared by induction melting under purified argon atmosphere. During the mechanical amorphization the grinded ingots were milled for different durations of time and with several interruptions in order to analyse the structure of the powders. The mechanical milling was performed in a Pulverisette5 high energy planetary ball-mill under argon atmosphere using stainless vial and balls with diameters of about 3 mm, 5 mm and 10 mm. The ball-to-powder ratio was 20:1. The milled powders were analyzed by XRD to determine the amorphous fraction, by SEM to characterize the microstructure and by DSC to observe processes in the powders during heating. After milling for 20 h, an amorphous structure appeared and the amorphous fraction was 95%.