A single-step method for the preparation of metastable ε-Fe3N nanoparticles by combustion of reactive gels containing iron nitrate (Fe(NO3)3) and hexamethylene-tetramine (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 ε-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 ferromag- netic behavior with a low-temperature magnetic moment of 1.09 μB/Fe, high room temperature saturation magnetization (∼80 emu/g), and low remanent magnetization (∼15 emu/g). The obtained value for the Curie temperature of ∼522 K is close to that (∼575 K) for bulk ε-Fe3N reported in the literature.
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