Thermal Plasma Synthesis of γ-FeN_x Nanoparticles as Precursors for the Fe₁₆N₂ Synthesis by Annealing

Abstract

An ordered Fe₁₆N₂ phase has been reported with iron moments as high as 3.2 μ_B. It is precipitated from nitrogen martensite structures ideally containing 10.5 at.% nitrogen. Due to the highly distorted crystal structure and metastability of this phase non-equilibrium processing routes are sought to synthesize this phase. Here we report on radio frequency (RF) plasma torch synthesis which is used to produce FeN. nanoparticles quenched into a body centered tetragonal bct) structure as precursors for further annealing studies to form α“- Fe₁₆N₂ phase. We have employed a Tekna PL-50 type 50 kW, RF plasma torch. A plasma gas mixture containing 40 standard liters per minute (slpm) Ar and 8 slpm Hydrogen - 70 slpm Ar gas was used as a sheath gas. Iron powder ( < 10 μm) was injected into the plasma stream using Ar flowing 15 slpm as a carrier gas. Nitrogen and Ammonia were used as a nitrogenization sources. Relatively low injection rates were used in order to achieve smaller particle sizes and thus faster quenching rates. We were able to produce particles containing up to 45 % of the quenched γ-phase. Observations based on x-ray diffraction (XRD) determination of lattice expansion and phase transition temperatures observed by differential thermal analysis (DTA) indicated that the quenched phase contains 6.5 atomic % nitrogen. Scherrer analysis of the fine particle broadening indicated that the average particle size for γ- phase is 27 nm, whereas this value is found to be 55 nm. for α-Fe. Nitrogen is well known for its grain size refinement in Fe thin films. Saturation magnetizations were found to be as low as 123 emu/g due to the presence of the nonmagnetic γ-FeN_x phase.