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Nanoscale Iron Nitride, ε-Fe3N: Preparation from liquid ammonia and magnetic Properties.

Zieschang, A.-M. and Bocarsly, Joshua D. and Duerrschnabel, Michael and Molina-Luna, Leopoldo and Kleebe, Hans-Joachim and Seshadri, Ram and Albert, B. R. (2017):
Nanoscale Iron Nitride, ε-Fe3N: Preparation from liquid ammonia and magnetic Properties.
29, In: Chemistry of Materials, (2), American Chemical Society, pp. 621-628, ISSN 0897-4756, DOI: 10.1021/acs.chemmater.6b04088,
[Article]

Abstract

ε-Fe3N shows interesting magnetism but is difficult to obtain as a pure and single-phase sample. We report a new preparation method using the reduction of iron(II) bromide with elemental sodium in liquid ammonia at −78 °C, followed by annealing at 573 K. Nanostructured and monophasic oxygen-free iron nitride, ε-Fe3N, is produced according to X-ray diffraction and transmission electron microscopy experiments. The magnetic properties between 2 and 625 K were characterized using a vibrating sample magnetometer, revealing soft ferromagnetic behavior with a low-temperature average moment of 1.5 μB/Fe and a Curie temperature of 500 K. TC is lower than that of bulk ε-Fe3N (575 K) [ Chem. Phys. Lett 2010, 493, 299], which corresponds well with the small particle size within the agglomerates (15.4 (±4.1) nm according to TEM, 15.8(1) according to XRD). Samples were analyzed before and after partial oxidation (Fe3N–FexOy core–shell nanoparticles with a 2–3 nm thick shell) by X-ray diffraction, transmission electron microscopy, electron energy-loss spectroscopy, and magnetic measurements. Both the pristine Fe3N nanoparticles and the oxidized core–shell particles showed shifting and broadening of the magnetic hysteresis loops upon cooling in a magnetic field.

Item Type: Article
Erschienen: 2017
Creators: Zieschang, A.-M. and Bocarsly, Joshua D. and Duerrschnabel, Michael and Molina-Luna, Leopoldo and Kleebe, Hans-Joachim and Seshadri, Ram and Albert, B. R.
Title: Nanoscale Iron Nitride, ε-Fe3N: Preparation from liquid ammonia and magnetic Properties.
Language: English
Abstract:

ε-Fe3N shows interesting magnetism but is difficult to obtain as a pure and single-phase sample. We report a new preparation method using the reduction of iron(II) bromide with elemental sodium in liquid ammonia at −78 °C, followed by annealing at 573 K. Nanostructured and monophasic oxygen-free iron nitride, ε-Fe3N, is produced according to X-ray diffraction and transmission electron microscopy experiments. The magnetic properties between 2 and 625 K were characterized using a vibrating sample magnetometer, revealing soft ferromagnetic behavior with a low-temperature average moment of 1.5 μB/Fe and a Curie temperature of 500 K. TC is lower than that of bulk ε-Fe3N (575 K) [ Chem. Phys. Lett 2010, 493, 299], which corresponds well with the small particle size within the agglomerates (15.4 (±4.1) nm according to TEM, 15.8(1) according to XRD). Samples were analyzed before and after partial oxidation (Fe3N–FexOy core–shell nanoparticles with a 2–3 nm thick shell) by X-ray diffraction, transmission electron microscopy, electron energy-loss spectroscopy, and magnetic measurements. Both the pristine Fe3N nanoparticles and the oxidized core–shell particles showed shifting and broadening of the magnetic hysteresis loops upon cooling in a magnetic field.

Journal or Publication Title: Chemistry of Materials
Volume: 29
Number: 2
Publisher: American Chemical Society
Divisions: 11 Department of Materials and Earth Sciences
11 Department of Materials and Earth Sciences > Earth Science
11 Department of Materials and Earth Sciences > Earth Science > Geo-Material-Science
11 Department of Materials and Earth Sciences > Material Science
11 Department of Materials and Earth Sciences > Material Science > Advanced Electron Microscopy (aem)
Date Deposited: 06 Dec 2018 10:20
DOI: 10.1021/acs.chemmater.6b04088
Funders: The work at Santa Barbara was supported by the MRSEC Program of the National Science Foundation under award no. DMR 1121053., J.D.B. is supported by the National Science Foundation Graduate Research Fellowship Program under grant no. 1650114., We also acknowledge financial support from the Hessen State Ministry of Higher Education, Research and the Arts via LOEWE RESPONSE., The transmission electron microscopes used in this work were partially funded by the German Research Foundation (DFG/INST163/2951).
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