Fe73.5-xCoxSi13.5B9Cu1Nb3
(x = 13.5 and 60 at.%) nanocrystalline alloys were studied by
means of x-ray diffraction, 57Fe Mössbauer spectrometry and
thermomagnetic measurements. For the first time, the
compositions of both the Fe, Co, Si nanocrystalline and the
residual amorphous phases were determined on the basis of
combined structural and magnetic hyperfine data. The Co content
of the nanocrystalline phase was found to be the same as the Co
content of the as-cast alloy. The hyperfine magnetic field
distribution of the intergranular phase shows the emergence of
a bimodal behaviour, consistent with a two-cluster-like model.
Such behaviour is attributed to the presence of iron-rich and
iron-poor zones located in the bulk of the intergranular region
and at the periphery of the crystalline grains, respectively.