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It has been shown according to the X-ray diffraction analysis that all alloys retain nanostructured state after the heat treatment. The appearance of sigma-phase was noted only for Fe52Cr48 alloy at annealing temperatures higher than 600C. The analysis of Mössbauer spectra, measured at room temperature, showed that the increase in annealing temperature of Fe70Cr30 and Fe60Cr40 samples leads to the phase separation (this phenomenon is also known as a spinodal decomposition) of a bcc solid solution of iron and chromium into two coherent phases: one of them is enriched in iron and the other is enriched with chromium.