In order to complete the research on the Fe–Se binary system, the phase structures with selenium contents from 50 to 60 at.% have been studied. Fe–Se binary samples used in this study were prepared by the high-temperature solid-state reaction method, and the phase structure of each sample was determined by powder X-ray diffraction. The solid solubility of the Fe3Se4 phase was determined to be from 56.1 to 57.6 at.% Se based on the values of unit-cell parameters. Magnetic properties of the samples were also studied.
