In Situ and Ex Situ X-ray Diffraction and Small-Angle X-ray Scattering Investigations of the Sol-Gel Synthesis of Fe3N and Fe3C

Matthew S Chambers, Robert D Hunter, Martin J Hollamby, Brian R Pauw, Andrew J Smith, Tim Snow, Ashleigh E Danks, Zoe Schnepp

Research output: Contribution to journalArticlepeer-review

Abstract

Iron nitride (Fe3N) and iron carbide (Fe3C) nanoparticles can be prepared via sol-gel synthesis. While sol-gel methods are simple, it can be difficult to control the crystalline composition, i.e., to achieve a Rietveld-pure product. In a previous in situ synchrotron study of the sol-gel synthesis of Fe3N/Fe3C, we showed that the reaction proceeds as follows: Fe3O4 → FeOx → Fe3N → Fe3C. There was considerable overlap between the different phases, but we were unable to ascertain whether this was due to the experimental setup (side-on heating of a quartz capillary which could lead to thermal gradients) or whether individual particle reactions proceed at different rates. In this paper, we use in situ wide- and small-angle X-ray scattering (wide-angle X-ray scattering (WAXS) and small-angle X-ray scattering (SAXS)) to demonstrate that the overlapping phases are indeed due to variable reaction rates. While the initial oxide nanoparticles have a small range of diameters, the size range expands considerably and very rapidly during the oxide-nitride transition. This has implications for the isolation of Rietveld-pure Fe3N, and in an extensive laboratory study, we were indeed unable to isolate phase-pure Fe3N. However, we made the surprising discovery that Rietveld-pure Fe3C nanoparticles can be produced at 500 °C with a sufficient furnace dwell time. This is considerably lower than the previous reports of the sol-gel synthesis of Fe3C nanoparticles.

Original languageEnglish
Pages (from-to)6742-6749
Number of pages8
JournalInorganic Chemistry
Volume61
Issue number18
Early online date26 Apr 2022
DOIs
Publication statusPublished - 9 May 2022

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