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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

Published online by Cambridge University Press:  29 April 2015

A. Harte*
Affiliation:
The University of Manchester, Manchester Materials Science Centre, Manchester M13 9PL, United Kingdom
T. Seymour
Affiliation:
The University of Manchester, Manchester Materials Science Centre, Manchester M13 9PL, United Kingdom
E.M. Francis
Affiliation:
The University of Manchester, Manchester Materials Science Centre, Manchester M13 9PL, United Kingdom
P. Frankel
Affiliation:
The University of Manchester, Manchester Materials Science Centre, Manchester M13 9PL, United Kingdom
S.P. Thompson
Affiliation:
Diamond Light Source, Didcot, Oxfordshire OX11 0DE, United Kingdom
D. Jädernäs
Affiliation:
Studsvik Nuclear AB, SE 611 82, Nyköping, Sweden
J. Romero
Affiliation:
Westinghouse Electric Company, Columbia, South Carolina, USA
L. Hallstadius
Affiliation:
Westinghouse Electric Sweden AB, SE 72163 Västerås, Sweden
M. Preuss
Affiliation:
The University of Manchester, Manchester Materials Science Centre, Manchester M13 9PL, United Kingdom
*
a) Address all correspondence to this author. e-mail: Allan.Harte@Manchester.ac.uk
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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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