The ball-milling of pure Fe and Zn elemental powders corresponding to
the Gamma-(Fe3Zn10), Gamma(1)-(Fe5Zn21), delta-(FeZn7), and zeta(FeZn1
3) compositions yields metastable crystalline phases. This is demonstr
ated by the peaks observed in the DSC measurements of the different ph
ases. These crystalline phases evolve differently with distinct or cha
racteristic stages with heat treatments. Cold-welding and powder agglo
meration are extensive, while the milled materials are completely homo
geneous.