In order to investigate the effect of the preparation technique on quasicrystal formation, amorphous (Zr0.585Ti0.082Cu0.142Ni0.114Al0.077)(100-x)Nb-x alloys with x = 2.5 and 5 at.% were produced by melt spinning and by ball milling of crystalline intermetallic compounds. The calorimetric and microstructure investigations revealed striking similarities between the differently synthesized samples. All the samples are characterized by a two-step crystallization process in which the first crystallization product does not depend on the way of preparation. In fact, the same metastable nanoscale quasicrystalline phase has been obtained by partial devitrification of ball-milled powders as well as of melt-spun ribbons. This demonstrates that ball milling is an alternative processing route to rapid solidification techniques for the preparation of quasicrystal-forming Zr-based alloys. (C) 2004 Kluwer Academic Publishers.