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Potentialities of Raman Imaging for the Analysis of Oxide Scales Formed on Zircaloy-4 and M5® in Air at High Temperature

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Abstract

Micro-Raman imaging was used to investigate oxide scales formed on Zircaloy-4 and M5® alloys in air, in the 800–1,000 °C temperature range. To create the 2D spectral images, the data were processed by different ways. The results clearly show that a microscopic picture of the scales in terms of microstructure and internal stresses can be developed from Raman spectral maps at the micron scale. Data on the microstructure, crystallography, and composition, are presented. They confirm that the crystallographic phases observed for the Zircaloy-4 and M5® alloys are different, since, for Zircaloy-4, we clearly observed additional Raman signatures which most probably track the presence of nitrogen in the layers well before the occurrence of the kinetic transition. In particular, they show the presence of cubic zirconia in the layers, and strongly suggest the presence of zirconium nitride and oxynitride. Results also suggest the presence of strong stress gradients in the oxide scales.

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Notes

  1. M5 is a trademark of AREVA, registered in France among other countries

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Acknowledgments

The authors acknowledge AREVA for their contribution to the support of this work. The authors also thank Bernard Guerin (CEZUS Paimboeuf) for the supply of the zircaloy samples, and Jean Desquines (IRSN) for many fruitful comments and discussions.

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Authors and Affiliations

  1. Institut de Radioprotection et de Sûreté Nucléaire (IRSN), Centre de Cadarache, 13115, St Paul lez Durance, France

    I. Idarraga & C. Duriez

  2. Laboratoire d’Electrochimie et de Physicochimie des Matériaux et des Interfaces (LEPMI), UMR 5279, CNRS – Grenoble INP – Université de Savoie – Université Joseph Fourier, BP75, 38402, Saint Martin d’Hères, France

    M. Mermoux

  3. Science et Ingénierie des Matériaux et Procédés (SIMaP), UMR 5266, CNRS – Grenoble INP – Université Joseph Fourier, BP75, 38402, Saint Martin d’Hères, France

    A. Crisci

  4. AREVA, AREVA NP Fuel Business Unit, 10 Rue Juliette Récamier, 69006, Lyon, France

    J. P. Mardon

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  1. I. Idarraga
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  2. M. Mermoux
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  3. C. Duriez
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  4. A. Crisci
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  5. J. P. Mardon
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Correspondence to M. Mermoux.

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Idarraga, I., Mermoux, M., Duriez, C. et al. Potentialities of Raman Imaging for the Analysis of Oxide Scales Formed on Zircaloy-4 and M5® in Air at High Temperature. Oxid Met 79, 289–302 (2013). https://doi.org/10.1007/s11085-012-9331-5

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  • DOI: https://doi.org/10.1007/s11085-012-9331-5

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