Fe-powders mechanically processed in a nitrogen environment were studi
ed by means of X-ray diffraction and chemical elemental analysis. Afte
r high-energy ball-milling, diffraction spectra exhibited shape modifi
cations consistent with the appearance of Fe-bct precipitates within t
he Fe-bcc matrix. The bet-phase accumulates monotonously with milling
time, constituting a source of inhomogeneous strains in the matrix. De
tailed analysis of diffraction spectra allowed the derivation of nitro
gen concentrations inside precipitates and matrix grains as well as in
the grain boundaries. The results obtained demonstrated for the first
time the nitrogen dynamics within a nanocrystalline microstructure at
different stages of mechanical processing.