Аннотация:The effect of temperature excitation on the structure and phase composition of an Fe3C/Fe7C3/П-phase/Cam composite obtained by mechanosynthesis of Fe–75 at % C has been studied by the methods ofX-ray diffraction, Mössbauer spectroscopy, thermogravimetric analysis, and differential scanning calorimetry. It is shown that the structural and phase variations at heating have a multistage character. In the temperature range 315–400°C crystallization of the paramagnetic П-phase with generation of Fe3C and/or Fe7C3occur. In the course of heating to higher temperatures, complete decomposition of carbide Fe7C3 (in the range 450–550°C) and partial decomposition of Fe3C (at 600°C and above) are observed. After cooling from 800–1000°C the mechanocomposite consists of α-Fe, cementite Fe3C, and graphite. The phase transformations are accompanied by the processes of composite oxidation with generation of Fe3O4 oxide and its subsequent reduction. The П-phase is a disorded amorphous carbide Fe1 – xCx, which is characterized by magnetic ordering at the temperature of liquid nitrogen.