A single-step method for the preparation of metastable epsilon-Fe3N nanoparticles by combustion of reactive gels containing iron nitrate (Fe(NO3)(3)) and hexamethylenetetramine (C6H12N4) in an inert atmosphere is reported. The results of Fourier transform infrared spectroscopy (FTIR) and thermal analysis coupled with dynamic mass spectrometry revealed that the exothermic decomposition of a coordination complex formed between Fe(NO3)(3) and HMTA is responsible for the formation of epsilon-Fe3N nanoscale particles with sizes of 5-15 nm. The magnetic properties between 5 and 350 K are characterized using a superconducting quantum interference device (SQUID) magnetometer, revealing a ferromagnetic behavior with a low-temperature magnetic moment of 1.09 mu(B)/Fe, high room temperature saturation magnetization (similar to 80 emu/g), and low remanent magnetization (similar to 15 emu/g). The obtained value for the Curie temperature of , similar to 522 K is close to that (similar to 575 K) for bulk epsilon-Fe3N reported in the literature.