The preparation of FeB by SHS in B2O3-Mg-Fe-Fe3O4 system was investigated in this study. In the preparation of FeB, the effects
of the initial pressure of inert gas in reactor, the content of Mg and Fe3O4 in mixture on the reactivity and reaction products was investigated. The minimum initial pressure of inert gas in reactor for SHS reaction in this system was 25 atm, and as the pressure increased, the concentration of unreacted Mg decreased and combustion temperature increased. At the initial inert gas pressure in reactor of 25 atm, the optimum composition for the preparation of pure FeB was 1.5B2O3+3.43Mg+1.7Fe+0.1Fe3O4. The FeB synthesized in this condition had an irregular shape and the particle size of 5 μm.