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Nanocrystalline alloys are prepared by controlled annealing of metallic glass precursors. The latter are obtained by rapid quenching of a melt on a rotating wheel. This process leads to structural deviation of the produced ribbons’ surfaces. Structural features of as-quenched and thermally annealed ⁵⁷Fe₈₁Mo₈Cu₁B₁₀ ribbons were studied employing Conversion Electron Mössbauer Spectrometry (CEMS) and Conversion X-ray Mössbauer Spectrometry (CXMS). Enrichment of the alloy’s composition in ⁵⁷Fe helped in identification of surface crystallites that were formed even during the production process. Magnetite and bcc-Fe were found at the wheel side of the as-quenched ribbons whereas only bcc-Fe nanocrystals were uncovered at the opposite air side. Accelerated formation of bcc-Fe was observed in this side of the ribbons after annealing. The relative content of magnetite at the wheel side was almost stable in near surface areas (CEMS) and in more deep subsurface regions (CXMS). It vanished completely after annealing at 550 °C. No magnetite was observed at the air side of the ribbons regardless the annealing temperature and/or depth of the scanned regions.