Joint reduction with hydrazine from aqueous solutions of precursors produced nanostructured powders of the Fe – Pt system in three characteristic phase regions. The samples were subjected to heat treatment in the range up to 800 ° C and characterized at all stages by X-ray diffraction and high-resolution electron microscopy; the elemental composition of the samples was refined by the method of optical emission spectroscopy with inductively coupled plasma. In the initially obtained samples, only a part of the substance is detected by diffraction-the largest, platinum-rich crystals with dimensions of about 10 nm (established from TEM images and broadening of diffraction lines). The fcc-type cubic lattice parameters and the composition of the observed crystals were estimated from the distances between the regular bands in TEM images, identified with atomic rows, based on the composition dependence of the bulk characteristics of mixed iron-platinum phases (according to ICDD databases). In the course of heating, the processes of phase transformation are traced in detail, the parameters of the resulting crystal structures of intermetallic compounds are fixed, and the mechanisms of these transformations are discussed. Based on the measured lattice parameters, the thermal expansion coefficients of some mixed phases are calculated and the phase compositions are estimated at different stages of heat treatment.