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Identification of the Zirconia Phases by Means of Raman Spectroscopy for Specimens Prepared by FIB Lift-Out Technique

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Abstract

The zirconium–zirconia interface that developed during high-temperature corrosion of pure zirconium was investigated. Samples were oxidized at 600 °C in air at atmospheric pressure. The oxidized sample was then prepared by means of focused ion beam (FIB) lift-out technique and examined using Raman spectroscopy technique in three different oxide zones (external, internal, and close to the metal–oxide interface). Structural investigation was performed using line mode Raman analysis. Implementation of these techniques revealed complexity of the studied system and confirmed the presence of a thin tetragonal sub-layer located in the proximity of the metal. Recorded Raman band displacements of monoclinic and tetragonal phases were interpreted in terms of stoichiometry level and compressive stress in the oxide. The thin layer of tetragonal phase is most likely characterized by lower amount of oxygen than the external part of the oxide.

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Acknowledgments

Financial support from Foundation for Polish Science through the HOMING PLUS/2013-8/7 program is gratefully acknowledged. The authors would like to thank the French embassy in Poland for funding one month internship (L. Kurpaska) at University of La Rochelle in the frame of “SSHN—séjour scientifique de haut niveau” program.

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Authors and Affiliations

  1. National Center for Nuclear Research, ST. A. Soltana 7/23, 05- 400, Otwock-Swierk, Poland

    Lukasz Kurpaska, Malgorzata Frelek-Kozak & Jacek Jagielski

  2. LaSIE UMR-CNRS 7356, Pole Science Et Technologie, Universite de La Rochelle, St. M Crepeau, 17042, La Rochelle Cedex, France

    Jean-Luc Grosseau-Poussard

  3. Institute of Electronic Materials Technology, St. Wolczynska 133, 01-919, Warsaw, Poland

    Iwona Jozwik & Jacek Jagielski

  4. Laboratoire Des Technologies Innovantes, Universite de Picardie Jules- Verne, 33 Rue St. Leu, 80039, Amiens Cedex, France

    Laurent Lahoche

  5. Laboratoire Roberval UMR 7337, Universite de Technologie de CompiegneCentre de Recherche de Royallieu, CS 60319, 60203, Compiegne Cedex, France

    Jerome Favergeon

Authors
  1. Lukasz Kurpaska
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  2. Malgorzata Frelek-Kozak
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  3. Jean-Luc Grosseau-Poussard
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  4. Iwona Jozwik
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  5. Laurent Lahoche
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  6. Jerome Favergeon
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  7. Jacek Jagielski
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Correspondence to Lukasz Kurpaska.

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Kurpaska, L., Frelek-Kozak, M., Grosseau-Poussard, JL. et al. Identification of the Zirconia Phases by Means of Raman Spectroscopy for Specimens Prepared by FIB Lift-Out Technique. Oxid Met 88, 521–530 (2017). https://doi.org/10.1007/s11085-016-9675-3

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  • DOI: https://doi.org/10.1007/s11085-016-9675-3

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