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Title: Nondestructive hydrogen analysis of steam-oxidized Zircaloy-4 by wide-angle neutron scattering

Abstract

In this study, a nondestructive neutron scattering method to precisely measure the hydrogen content in high-temperature steam-oxidized Zircaloy-4 cladding was developed. Zircaloy-4 cladding was used to produce hydrided specimens with hydrogen content up to ≈500 wppm. Following hydrogen charging, the hydrogen content of the hydrided specimens was measured using the vacuum hot extraction method, by which the samples with desired hydrogen concentrations were selected for the neutron study. The hydrided samples were then oxidized in steam up to ≈6.0wt. % at 1100°C. Optical microscopy shows that our hydriding procedure results in uniform distribution of circumferential hydrides across the wall thickness, and uniform oxide layers were formed on the sample surfaces by the steam oxidation. Small- and wide-angle neutron scattering were simultaneously performed to provide a quick (less than an hour per sample) measurement of the hydrogen content in various types of hydrided and oxidized Zircaloy-4. Our study demonstrates that the hydrogen in pre-oxidized Zircaloy-4 cladding can be measured very accurately by both small- and wide-angle neutron scattering. For steam-oxidized samples, the small-angle neutron scattering is contaminated with coherent scattering from additional structural features induced by the steam oxidation. However, the scattering intensity of the wide-angle neutron scattering increases proportionally withmore » the hydrogen charged in the samples. The hydrogen content and wide-angle neutron scattering intensity are highly linearly correlated for the oxidized cladding samples examined in this work, and can be used to precisely determine the hydrogen content in steam-oxidized Zircaloy-4 samples. Hydrogen contents determined by neutron scattering of oxidation samples were also found to be consistent with the results of chemical analysis within acceptable margins for error.« less

Authors:
ORCiD logo [1]; ORCiD logo [1];  [1];  [1]; ORCiD logo [1]
  1. Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)
Publication Date:
Research Org.:
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Biological and Environmental Research (BER)
OSTI Identifier:
1427643
Grant/Contract Number:  
AC05-00OR22725
Resource Type:
Accepted Manuscript
Journal Name:
Journal of Nuclear Materials
Additional Journal Information:
Journal Volume: 502; Journal Issue: C; Journal ID: ISSN 0022-3115
Publisher:
Elsevier
Country of Publication:
United States
Language:
English
Subject:
71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSICS; 42 ENGINEERING; 36 MATERIALS SCIENCE

Citation Formats

Yan, Yong, Qian, Shuo, Garrison, Ben, Smith, Tyler, and Kim, Peter. Nondestructive hydrogen analysis of steam-oxidized Zircaloy-4 by wide-angle neutron scattering. United States: N. p., 2018. Web. doi:10.1016/j.jnucmat.2018.02.016.
Yan, Yong, Qian, Shuo, Garrison, Ben, Smith, Tyler, & Kim, Peter. Nondestructive hydrogen analysis of steam-oxidized Zircaloy-4 by wide-angle neutron scattering. United States. https://doi.org/10.1016/j.jnucmat.2018.02.016
Yan, Yong, Qian, Shuo, Garrison, Ben, Smith, Tyler, and Kim, Peter. Sun . "Nondestructive hydrogen analysis of steam-oxidized Zircaloy-4 by wide-angle neutron scattering". United States. https://doi.org/10.1016/j.jnucmat.2018.02.016. https://www.osti.gov/servlets/purl/1427643.
@article{osti_1427643,
title = {Nondestructive hydrogen analysis of steam-oxidized Zircaloy-4 by wide-angle neutron scattering},
author = {Yan, Yong and Qian, Shuo and Garrison, Ben and Smith, Tyler and Kim, Peter},
abstractNote = {In this study, a nondestructive neutron scattering method to precisely measure the hydrogen content in high-temperature steam-oxidized Zircaloy-4 cladding was developed. Zircaloy-4 cladding was used to produce hydrided specimens with hydrogen content up to ≈500 wppm. Following hydrogen charging, the hydrogen content of the hydrided specimens was measured using the vacuum hot extraction method, by which the samples with desired hydrogen concentrations were selected for the neutron study. The hydrided samples were then oxidized in steam up to ≈6.0wt. % at 1100°C. Optical microscopy shows that our hydriding procedure results in uniform distribution of circumferential hydrides across the wall thickness, and uniform oxide layers were formed on the sample surfaces by the steam oxidation. Small- and wide-angle neutron scattering were simultaneously performed to provide a quick (less than an hour per sample) measurement of the hydrogen content in various types of hydrided and oxidized Zircaloy-4. Our study demonstrates that the hydrogen in pre-oxidized Zircaloy-4 cladding can be measured very accurately by both small- and wide-angle neutron scattering. For steam-oxidized samples, the small-angle neutron scattering is contaminated with coherent scattering from additional structural features induced by the steam oxidation. However, the scattering intensity of the wide-angle neutron scattering increases proportionally with the hydrogen charged in the samples. The hydrogen content and wide-angle neutron scattering intensity are highly linearly correlated for the oxidized cladding samples examined in this work, and can be used to precisely determine the hydrogen content in steam-oxidized Zircaloy-4 samples. Hydrogen contents determined by neutron scattering of oxidation samples were also found to be consistent with the results of chemical analysis within acceptable margins for error.},
doi = {10.1016/j.jnucmat.2018.02.016},
journal = {Journal of Nuclear Materials},
number = C,
volume = 502,
place = {United States},
year = {Sun Apr 15 00:00:00 EDT 2018},
month = {Sun Apr 15 00:00:00 EDT 2018}
}

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