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Abstract The structure, phase and chemical compositions of surface layers in different depths of Fe-3%Si alloy were investigated. According to the X-ray Photoelectron Spectroscopy (XPS) spectrum (penetration depth of up to ≈1 nm) of the as-prepared sample, a layer of SiO2 was present on the top. After the subsequent Ar+ sputtering (removing the SiO2 layer), a segregation of Si atoms and two other phases were observed. The phases were described as the cubic c-FeSi and Fe3Si. The emission 57Fe Mossbauer spectra confirmed a presence of these phases. The α-Fe and solid solution of α-Fe + 1wt.%Si were recognized in the Conversion Electron Mossbauer spectra (penetration depth ≈ 300 nm) while the Mossbauer spectra taken in scattering geometry with detection of 14.4 keV gamma radiation (scanning depth of ≈30 µm) indicate Fe-3wt.%Si solid solution as a main phase. [ABSTRACT FROM AUTHOR]