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Advances in synchrotron x-ray diffraction and transmission electron microscopy techniques for the investigation of microstructure evolution in proton- and neutron-irradiated zirconium alloys

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Abstract

Transmission electron microscopy (TEM) studies provide mechanistic understanding of nanoscale processes, whereas advanced synchrotron XRD (SXRD) enables precise measurements on volumes that are more representative of bulk materials. Therefore, the combined strengths of these techniques can provide new insight into irradiation-induced mechanistic processes. In the present study, their application to Zircaloy-2, proton-irradiated to 2.3, 4.7, and 7.0 dpa at 2 MeV and 350 °C and neutron-irradiated to 9.5 and 13.1 × 1025 n m−2 are exemplified. The application of correlative spectral imaging and structural TEM investigations to the phase transformation of Zr(Fe,Nb)2 precipitates in Low-Sn ZIRLO™, neutron-irradiated to 8.9–9 × 1025 n m−2, demonstrates the possibility of a Cr core nucleation site. Anomalous broadening is observed in SXRD profiles, which is believed to be caused by defect clusters and precursors to dislocation loop nucleation. The challenges to quantitative analysis of dislocations by SXRD are highlighted with reference to the segregation of Fe and Ni to basal planes and dislocation cores, observed by spectral imaging in the TEM.

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ACKNOWLEDGMENTS

This work is funded by an EPSRC Leadership Fellowship for the study of irradiation damage in zirconium alloys, and is supported heavily from industrial contributors and especially Westinghouse and Studsvik in terms of both material acquisition and useful discussions. The authors would like to thank Matthew Topping for useful discussions, Gary Was and Ovidiu Toader at the Michigan Ion Beam Laboratory for the use of their facility in the proton irradiation experiments, and the experimental officers at Diamond light source for their aid in implementing the SXRD experiments.

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Authors and Affiliations

  1. Manchester Materials Science Centre, The University of Manchester, Manchester, M13 9PL, UK

    A. Harte, T. Seymour, E. M. Francis, P. Frankel & M. Preuss

  2. Diamond Light Source, Didcot, Oxfordshire, OX11 0DE, UK

    S. P. Thompson

  3. Studsvik Nuclear AB, SE, 611 82, Nyköping, Sweden

    D. Jädernäs

  4. Westinghouse Electric Company, Columbia, South Carolina, USA

    J. Romero

  5. Westinghouse Electric Sweden AB, SE, 72163, Västerås, Sweden

    L. Hallstadius

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  1. A. Harte
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Harte, A., Seymour, T., Francis, E.M. et al. Advances in synchrotron x-ray diffraction and transmission electron microscopy techniques for the investigation of microstructure evolution in proton- and neutron-irradiated zirconium alloys. Journal of Materials Research 30, 1349–1365 (2015). https://doi.org/10.1557/jmr.2015.65

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