Local and long-range atomic/magnetic structure of non-stoichiometric spinel iron oxide nanocrystallites

Andersen, Henrik L.; Frandsen, Benjamin A.; Gunnlaugsson, Haraldur P.; Jørgensen, Mads R. V.; Billinge, Simon J. L.; Jensen, Kirsten M. Ø.; Christensen, Mogens

doi:10.1107/S2052252520013585

Local and long-range atomic/magnetic structure of non-stoichiometric spinel iron oxide nanocrystallites

Journal Article · Fri Jan 01 00:00:00 EST 2021 · IUCrJ

DOI:https://doi.org/10.1107/S2052252520013585· OSTI ID:1712508

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Spinel iron oxide nanoparticles of different mean sizes in the range 10–25 nm have been prepared by surfactant-free up-scalable near- and super-critical hydrothermal synthesis pathways and characterized using a wide range of advanced structural characterization methods to provide a highly detailed structural description. The atomic structure is examined by combined Rietveld analysis of synchrotron powder X-ray diffraction (PXRD) data and time-of-flight neutron powder-diffraction (NPD) data. The local atomic ordering is further analysed by pair distribution function (PDF) analysis of both X-ray and neutron total-scattering data. It is observed that a non-stoichiometric structural model based on a tetragonal γ-Fe ₂ O ₃ phase with vacancy ordering in the structure (space group P 4 ₃ 2 ₁ 2) yields the best fit to the PXRD and total-scattering data. Detailed peak-profile analysis reveals a shorter coherence length for the superstructure, which may be attributed to the vacancy-ordered domains being smaller than the size of the crystallites and/or the presence of anti-phase boundaries, faulting or other disorder effects. The intermediate stoichiometry between that of γ-Fe ₂ O ₃ and Fe ₃ O ₄ is confirmed by refinement of the Fe/O stoichiometry in the scattering data and quantitative analysis of Mössbauer spectra. The structural characterization is complemented by nano/micro-structural analysis using transmission electron microscopy (TEM), elemental mapping using scanning TEM, energy-dispersive X-ray spectroscopy and the measurement of macroscopic magnetic properties using vibrating sample magnetometry. Notably, no evidence is found of a Fe ₃ O ₄ /γ-Fe ₂ O ₃ core-shell nanostructure being present, which had previously been suggested for non-stoichiometric spinel iron oxide nanoparticles. Finally, the study is concluded using the magnetic PDF (mPDF) method to model the neutron total-scattering data and determine the local magnetic ordering and magnetic domain sizes in the iron oxide nanoparticles. The mPDF data analysis reveals ferrimagnetic collinear ordering of the spins in the structure and the magnetic domain sizes to be ∼60–70% of the total nanoparticle sizes. The present study is the first in which mPDF analysis has been applied to magnetic nanoparticles, establishing a successful precedent for future studies of magnetic nanoparticles using this technique.

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Research Organization:: Brookhaven National Laboratory (BNL), Upton, NY (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: AC05-00OR22725; SC0012704

OSTI ID:: 1712508

Alternate ID(s):: OSTI ID: 1756299

Report Number(s):: BNL--220778-2021-JAAM; PII: S2052252520013585

Journal Information:: IUCrJ, Journal Name: IUCrJ Journal Issue: 1 Vol. 8; ISSN 2052-2525; ISSN IUCRAJ

Publisher:: International Union of CrystallographyCopyright Statement

Country of Publication:: United Kingdom

Language:: English

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SUPERCONDUCTIVITY AND SUPERFLUIDITY
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Local and long-range atomic/magnetic structure of non-stoichiometric spinel iron oxide nanocrystallites

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