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

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 → FeO_x → 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.

SUBMITTER: Chambers MS

PROVIDER: S-EPMC9092341 | biostudies-literature | 2022 May

REPOSITORIES: biostudies-literature

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

Chambers Matthew S MS Hunter Robert D RD Hollamby Martin J MJ Pauw Brian R BR Smith Andrew J AJ Snow Tim T Danks Ashleigh E AE Schnepp Zoe Z

Inorganic chemistry 20220426 18

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 → Fe3 ...[more]

PMID: 35471920

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Dataset Information

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

Publications

<i>In Situ</i> and <i>Ex Situ</i> X-ray Diffraction and Small-Angle X-ray Scattering Investigations of the Sol-Gel Synthesis of Fe<sub>3</sub>N and Fe<sub>3</sub>C.

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