Abstract
Polymer-derived SiCN ceramics, annealed (also referred to as pyrolyzed) at 1000, 1100, and 1285 °C, and doped with Fe(III) acetylacetonate, are investigated by electron paramagnetic resonance (EPR) from 4 to 120 K at X-band (9.425 GHz). In addition, the SiCN ceramic, annealed at 1100 °C, was studied by EPR at 300 K at W-band (93.96 GHz). There was observed a significant increase in EPR linewidth due to dangling bonds (g = 2.001) below 20 K at X-band. The low-field X-band FMR line (g ≈ 12) indicated the presence of ferromagnetic Fe5Si3 crystallites. There were found two EPR lines due to carbon-related dangling bonds: (1) those present as defects on the surface of the free-carbon phase (as sp2 carbon-related dangling bonds with g = 2.0011) and (2) those present within the bulk of carbon phase (as sp3 carbon-related dangling bonds with g = 2.0033). On the other hand, the intense low-field EPR signal observed at X-band was not observed at W-band. As well, there was observed splitting of the single broad EPR signal observed at g = 2.05 at X-band into two signals at W-band at g = 1.99 and g = 2.06, due to two different Fe-containing superparamagnetic nanocrystallites. Two new EPR signals, not observed at X-band, were observed at W-band, namely at g = 2.28 and g = 3.00, which are also due to g∥ of these superparamagnetic nanocrystallites.
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Acknowledgements
This research was supported by the Natural Sciences and Engineering Research Council of Canada (NSERC) (SKM); SIA is grateful to Ministry of Education and Science of Russian Federation, for partial support in the frame of research project, allocated to Kazan Federal University for the state assignment in the sphere of scientific activities (#3.2166.2017/4.6). SIA is grateful to Dr. S. B. Orlinskii for high-frequency (W-band) EPR measurements at the Federal Center of Shared Facilities of Kazan Federal University.
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Andronenko, S.I., Rodionov, A.A. & Misra, S.K. A Variable Temperature X- and W-Band EPR Study of Fe-Doped SiCN Ceramics Annealed at 1000, 1100, and 1285 °C: Dangling Bonds, Ferromagnetism and Superparamagnetism. Appl Magn Reson 49, 335–344 (2018). https://doi.org/10.1007/s00723-017-0973-y
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DOI: https://doi.org/10.1007/s00723-017-0973-y