The process of mechanical alloying consists of intimate mixing and mec
hanical working of elemental powders in a high-energy ball mill. It ha
s been well established that this process is able to produce nanocryst
alline and amorphous material. In this study, the structural effects o
f mechanical alloying of pure Fe, Fe50W50 and Fe50Mo50 powders were in
vestigated by X-ray diffraction and Mossbauer spectroscopy. For all ca
ses, nanocrystalline and/or amorphous fractions were found after milli
ng. The resulting particle size was determined by X-ray diffraction. P
ure Fe does not amorphize even after prolonged milling times. For the
nanocrystalline powder, significant changes in the linewidth and the h
yperfine field are found. Powder mixtures of Fe50Mo50 and Fe50W50 are
completely amorphous after milling times of 10 h, as seen by Mossbauer
spectroscopy, but nanocrystalline fractions of the non-iron part are
still found in X-ray diffraction. Also in the amorphous state, further
changes in the hyperfine parameters are found with increasing milling
time.