We synthesized submicron-sized "-Fe x N (2 5 x 5 3) particles by heating 180-nm Fe 3 O 4 particles in an atmosphere of NH 3 , both with and without H 2 , and we studied their structural and magnetic properties. The nitride samples (first step nitridation) prepared by NH 3 and annealed at 623 K ("-Fe 2 N) had an expanded unit cell and were paramagnetic at room temperature. The purpose of H 2 annealing, which was successively applied on the first step nitride sample, was to dissolve excess nitrogen atoms and reduce the lattice constant. The nitrogen concentrations were estimated from X-ray diffraction patterns. Saturation magnetization was found to increase with the H 2 annealing time. The nitrogen diffusion constant in the submicron hcp particles was found to be 6:33 Â 10 À20 m 2 /s, which is about three orders of magnitude smaller than that of the bulk hcp iron nitrides. This may result from the coating materials, such as SiO 2 and others, covering the inner core nitrides, where nitrogen atoms passed through during diffusion.