Abstract: To explore the reaction behavior of trace oxygen during the flash combustion process of falling FeSi75 powder in a nitrogen flow, a flash-combustion-synthesized Fe-Si₃N₄ sample was heat-treated to remove SiO₂. The samples before and after the treatment were investigated by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy, and the formation mechanism of SiO₂ was investigated. The results show that SiO₂ in the Fe-Si₃N₄ is mainly located on the surface or around the Si₃N₄ particles in dense areas, existing in both crystalline and amorphous states; when the FeSi75 particles, which are less than 0.074 mm in size, fell in up-flowing hot N₂ stream, trace oxygen in the N₂ stream did not significantly hinder the nitridation of FeSi75 particles as it was consumed by the surface oxidation of the generated Si₃N₄ particles to form SiO₂. At the reaction zone, the oxidation of Si₃N₄ particles decreased the oxygen partial pressure in the N₂ stream and greatly reduced the opportunity for FeSi75 particles to be oxidized into SiO₂; by virtue of the SiO₂ film developed on the surface, the Si₃N₄ particles adhered to each other and formed dense areas in the material.