Synthesis, morphology, thermal stability and magnetic properties of α″-Fe16N2 nanoparticles obtained by hydrogen reduction of γ-Fe2O3 and subsequent nitrogenation

Abstract

Typical synthesis of α″-Fe16N2 nanoparticles involves reduction of iron oxides by hydrogen at elevated temperatures which is disadvantageous due to the particle coalescence. Here we report on a process for reduction of iron oxides at elevated pressures and show that by increasing hydrogen pressure from atmospheric to 53 MPa, it is possible to reduce the reaction temperature from 663 K down to 483 K, resulting in phase-pure α-Fe nanoparticles without noticeable particle growth. By subsequent nitrogenation in an ammonia flow, fine, 99% phase-pure α″-Fe16N2 nanoparticles could be synthesized. The reduction temperature and the respective particle size has a significant influence on the nitrogenation step. α″-Fe16N2 nanoparticles exhibit semi-hard magnetic properties with Ms(0) = 215 Am2 kg−1, μ0Hc = 0.22 T, TC = 634 K and exchange stiffness Ac = 6.84 pJ m−1, Aa,b = 7.53 pJ m−1. Synthesis conditions, microstructure, chemical composition and thermal stability of the nanoparticles are systematically studied and correlated with the observed magnetic properties.