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

Yong Yan, Shuo Qian, Ben Garrison, Tyler Smith, Peter Kim

Research output: Contribution to journalArticlepeer-review

3 Scopus citations

Abstract

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 ≈6.0 wt. % 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.

Original languageEnglish
Pages (from-to)191-200
Number of pages10
JournalJournal of Nuclear Materials
Volume502
DOIs
StatePublished - Apr 15 2018

Funding

This manuscript was authored by UT-Battelle, LLC, under contract DE-AC05-00OR22725 with the US Department of Energy (DOE). The US government retains and the publisher, by accepting the article for publication, acknowledges that the US government retains a nonexclusive, paid-up, irrevocable, worldwide license to publish or reproduce the published form of this manuscript, or allow others to do so, for US government purposes. DOE will provide public access to these results of federally sponsored research in accordance with the DOE Public Access Plan ( http://energy.gov/downloads/doe-public-access-plan ). This research used resources at the High Flux Isotope Reactor, a US Department of Energy (DOE) Office of Science User Facility operated by the Oak Ridge National Laboratory. The CG3 instrument is supported by the DOE Office of Biological and Environmental Research. We would like to thank Douglas Armitage for designing the sample holder and stage in this experiment.

Fingerprint

Dive into the research topics of 'Nondestructive hydrogen analysis of steam-oxidized Zircaloy-4 by wide-angle neutron scattering'. Together they form a unique fingerprint.

Cite this