Chemical and elemental mapping of spent nuclear fuel sections by soft X‐ray spectromicroscopy
Soft X‐ray spectromicroscopy at the O K‐edge, U N4,5‐edges and Ce M4,5‐edges has been performed on focused ion beam sections of spent nuclear fuel for the first time, yielding chemical information on the sub‐micrometer scale. To analyze these data, a modification to non‐negative matrix factorization...
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| Published in | Journal of synchrotron radiation Vol. 29; no. 1; pp. 67 - 79 |
|---|---|
| Main Authors | , , , , , , , , , |
| Format | Journal Article |
| Language | English |
| Published |
5 Abbey Square, Chester, Cheshire CH1 2HU, England
International Union of Crystallography
01.01.2022
John Wiley & Sons, Inc International Union of Crystallography (IUCr) |
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| Online Access | Get full text |
| ISSN | 1600-5775 0909-0495 1600-5775 |
| DOI | 10.1107/S1600577521012315 |
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| Abstract | Soft X‐ray spectromicroscopy at the O K‐edge, U N4,5‐edges and Ce M4,5‐edges has been performed on focused ion beam sections of spent nuclear fuel for the first time, yielding chemical information on the sub‐micrometer scale. To analyze these data, a modification to non‐negative matrix factorization (NMF) was developed, in which the data are no longer required to be non‐negative, but the non‐negativity of the spectral components and fit coefficients is largely preserved. The modified NMF method was utilized at the O K‐edge to distinguish between two components, one present in the bulk of the sample similar to UO2 and one present at the interface of the sample which is a hyperstoichiometric UO2+x species. The species maps are consistent with a model of a thin layer of UO2+x over the entire sample, which is likely explained by oxidation after focused ion beam (FIB) sectioning. In addition to the uranium oxide bulk of the sample, Ce measurements were also performed to investigate the oxidation state of that fission product, which is the subject of considerable interest. Analysis of the Ce spectra shows that Ce is in a predominantly trivalent state, with a possible contribution from tetravalent Ce. Atom probe analysis was performed to provide confirmation of the presence and localization of Ce in the spent fuel.
Soft X‐ray spectromicroscopy at the O K‐edge, U N4,5‐edges and Ce M4,5‐edges has been performed on focused ion beam sections of spent nuclear fuel for the first time. Analysis of oxygen spectra using a modified non‐negative matrix factorization method is consistent with a thin layer of hyperstoichiometric uranium oxide having been formed at the interface of a sample consisting of primarily UO2, probably formed after sample preparation. The cerium oxidation state is shown to be predominantly trivalent, with a possible small contribution from tetravalent Ce. |
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| AbstractList | Soft X-ray spectromicroscopy at the O
K
-edge, U
N
4,5
-edges and Ce
M
4,5
-edges has been performed on focused ion beam sections of spent nuclear fuel for the first time, yielding chemical information on the sub-micrometer scale. To analyze these data, a modification to non-negative matrix factorization (NMF) was developed, in which the data are no longer required to be non-negative, but the non-negativity of the spectral components and fit coefficients is largely preserved. The modified NMF method was utilized at the O
K
-edge to distinguish between two components, one present in the bulk of the sample similar to UO
2
and one present at the interface of the sample which is a hyperstoichiometric UO
2+
x
species. The species maps are consistent with a model of a thin layer of UO
2+
x
over the entire sample, which is likely explained by oxidation after focused ion beam (FIB) sectioning. In addition to the uranium oxide bulk of the sample, Ce measurements were also performed to investigate the oxidation state of that fission product, which is the subject of considerable interest. Analysis of the Ce spectra shows that Ce is in a predominantly trivalent state, with a possible contribution from tetravalent Ce. Atom probe analysis was performed to provide confirmation of the presence and localization of Ce in the spent fuel. Soft X-ray spectromicroscopy at the O K-edge, U N4,5-edges and Ce M4,5-edges has been performed on focused ion beam sections of spent nuclear fuel for the first time, yielding chemical information on the sub-micrometer scale. To analyze these data, a modification to non-negative matrix factorization (NMF) was developed, in which the data are no longer required to be non-negative, but the non-negativity of the spectral components and fit coefficients is largely preserved. The modified NMF method was utilized at the O K-edge to distinguish between two components, one present in the bulk of the sample similar to UO2 and one present at the interface of the sample which is a hyperstoichiometric UO2+x species. The species maps are consistent with a model of a thin layer of UO2+x over the entire sample, which is likely explained by oxidation after focused ion beam (FIB) sectioning. In addition to the uranium oxide bulk of the sample, Ce measurements were also performed to investigate the oxidation state of that fission product, which is the subject of considerable interest. Analysis of the Ce spectra shows that Ce is in a predominantly trivalent state, with a possible contribution from tetravalent Ce. Atom probe analysis was performed to provide confirmation of the presence and localization of Ce in the spent fuel. Soft X-ray spectromicroscopy at the O K-edge, U N4,5-edges and Ce M4,5-edges has been performed on focused ion beam sections of spent nuclear fuel for the first time, yielding chemical information on the sub-micrometer scale. To analyze these data, a modification to non-negative matrix factorization (NMF) was developed, in which the data are no longer required to be non-negative, but the non-negativity of the spectral components and fit coefficients is largely preserved. The modified NMF method was utilized at the O K-edge to distinguish between two components, one present in the bulk of the sample similar to UO2 and one present at the interface of the sample which is a hyperstoichiometric UO2+x species. The species maps are consistent with a model of a thin layer of UO2+x over the entire sample, which is likely explained by oxidation after focused ion beam (FIB) sectioning. In addition to the uranium oxide bulk of the sample, Ce measurements were also performed to investigate the oxidation state of that fission product, which is the subject of considerable interest. Analysis of the Ce spectra shows that Ce is in a predominantly trivalent state, with a possible contribution from tetravalent Ce. Atom probe analysis was performed to provide confirmation of the presence and localization of Ce in the spent fuel.Soft X-ray spectromicroscopy at the O K-edge, U N4,5-edges and Ce M4,5-edges has been performed on focused ion beam sections of spent nuclear fuel for the first time, yielding chemical information on the sub-micrometer scale. To analyze these data, a modification to non-negative matrix factorization (NMF) was developed, in which the data are no longer required to be non-negative, but the non-negativity of the spectral components and fit coefficients is largely preserved. The modified NMF method was utilized at the O K-edge to distinguish between two components, one present in the bulk of the sample similar to UO2 and one present at the interface of the sample which is a hyperstoichiometric UO2+x species. The species maps are consistent with a model of a thin layer of UO2+x over the entire sample, which is likely explained by oxidation after focused ion beam (FIB) sectioning. In addition to the uranium oxide bulk of the sample, Ce measurements were also performed to investigate the oxidation state of that fission product, which is the subject of considerable interest. Analysis of the Ce spectra shows that Ce is in a predominantly trivalent state, with a possible contribution from tetravalent Ce. Atom probe analysis was performed to provide confirmation of the presence and localization of Ce in the spent fuel. Soft X‐ray spectromicroscopy at the O K‐edge, U N4,5‐edges and Ce M4,5‐edges has been performed on focused ion beam sections of spent nuclear fuel for the first time, yielding chemical information on the sub‐micrometer scale. To analyze these data, a modification to non‐negative matrix factorization (NMF) was developed, in which the data are no longer required to be non‐negative, but the non‐negativity of the spectral components and fit coefficients is largely preserved. The modified NMF method was utilized at the O K‐edge to distinguish between two components, one present in the bulk of the sample similar to UO2 and one present at the interface of the sample which is a hyperstoichiometric UO2+x species. The species maps are consistent with a model of a thin layer of UO2+x over the entire sample, which is likely explained by oxidation after focused ion beam (FIB) sectioning. In addition to the uranium oxide bulk of the sample, Ce measurements were also performed to investigate the oxidation state of that fission product, which is the subject of considerable interest. Analysis of the Ce spectra shows that Ce is in a predominantly trivalent state, with a possible contribution from tetravalent Ce. Atom probe analysis was performed to provide confirmation of the presence and localization of Ce in the spent fuel. Soft X‐ray spectromicroscopy at the O K‐edge, U N4,5‐edges and Ce M4,5‐edges has been performed on focused ion beam sections of spent nuclear fuel for the first time, yielding chemical information on the sub‐micrometer scale. To analyze these data, a modification to non‐negative matrix factorization (NMF) was developed, in which the data are no longer required to be non‐negative, but the non‐negativity of the spectral components and fit coefficients is largely preserved. The modified NMF method was utilized at the O K‐edge to distinguish between two components, one present in the bulk of the sample similar to UO2 and one present at the interface of the sample which is a hyperstoichiometric UO2+x species. The species maps are consistent with a model of a thin layer of UO2+x over the entire sample, which is likely explained by oxidation after focused ion beam (FIB) sectioning. In addition to the uranium oxide bulk of the sample, Ce measurements were also performed to investigate the oxidation state of that fission product, which is the subject of considerable interest. Analysis of the Ce spectra shows that Ce is in a predominantly trivalent state, with a possible contribution from tetravalent Ce. Atom probe analysis was performed to provide confirmation of the presence and localization of Ce in the spent fuel. Soft X‐ray spectromicroscopy at the O K‐edge, U N4,5‐edges and Ce M4,5‐edges has been performed on focused ion beam sections of spent nuclear fuel for the first time. Analysis of oxygen spectra using a modified non‐negative matrix factorization method is consistent with a thin layer of hyperstoichiometric uranium oxide having been formed at the interface of a sample consisting of primarily UO2, probably formed after sample preparation. The cerium oxidation state is shown to be predominantly trivalent, with a possible small contribution from tetravalent Ce. Soft X-ray spectromicroscopy at the O K-edge, U N -edges and Ce M -edges has been performed on focused ion beam sections of spent nuclear fuel for the first time, yielding chemical information on the sub-micrometer scale. To analyze these data, a modification to non-negative matrix factorization (NMF) was developed, in which the data are no longer required to be non-negative, but the non-negativity of the spectral components and fit coefficients is largely preserved. The modified NMF method was utilized at the O K-edge to distinguish between two components, one present in the bulk of the sample similar to UO and one present at the interface of the sample which is a hyperstoichiometric UO species. The species maps are consistent with a model of a thin layer of UO over the entire sample, which is likely explained by oxidation after focused ion beam (FIB) sectioning. In addition to the uranium oxide bulk of the sample, Ce measurements were also performed to investigate the oxidation state of that fission product, which is the subject of considerable interest. Analysis of the Ce spectra shows that Ce is in a predominantly trivalent state, with a possible contribution from tetravalent Ce. Atom probe analysis was performed to provide confirmation of the presence and localization of Ce in the spent fuel. Soft X-ray spectromicroscopy at the O K -edge, U N 4,5 -edges and Ce M 4,5 -edges has been performed on focused ion beam sections of spent nuclear fuel for the first time. Analysis of oxygen spectra using a modified non-negative matrix factorization method is consistent with a thin layer of hyperstoichiometric uranium oxide having been formed at the interface of a sample consisting of primarily UO 2 , probably formed after sample preparation. The cerium oxidation state is shown to be predominantly trivalent, with a possible small contribution from tetravalent Ce. Soft X-ray spectromicroscopy at the O K -edge, U N 4,5 -edges and Ce M 4,5 -edges has been performed on focused ion beam sections of spent nuclear fuel for the first time, yielding chemical information on the sub-micrometer scale. To analyze these data, a modification to non-negative matrix factorization (NMF) was developed, in which the data are no longer required to be non-negative, but the non-negativity of the spectral components and fit coefficients is largely preserved. The modified NMF method was utilized at the O K -edge to distinguish between two components, one present in the bulk of the sample similar to UO 2 and one present at the interface of the sample which is a hyperstoichiometric UO 2+ x species. The species maps are consistent with a model of a thin layer of UO 2+ x over the entire sample, which is likely explained by oxidation after focused ion beam (FIB) sectioning. In addition to the uranium oxide bulk of the sample, Ce measurements were also performed to investigate the oxidation state of that fission product, which is the subject of considerable interest. Analysis of the Ce spectra shows that Ce is in a predominantly trivalent state, with a possible contribution from tetravalent Ce. Atom probe analysis was performed to provide confirmation of the presence and localization of Ce in the spent fuel. |
| Author | Mara, Michael W. Smiles, Danil E. Altman, Alison B. Bachhav, Mukesh Lussier, Daniel He, Lingfeng Shuh, David K. Degueldre, Claude Minasian, Stefan G. Ditter, Alexander Scott |
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| BackLink | https://www.ncbi.nlm.nih.gov/pubmed/34985424$$D View this record in MEDLINE/PubMed https://www.osti.gov/biblio/1837324$$D View this record in Osti.gov |
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| CitedBy_id | crossref_primary_10_1116_6_0001880 crossref_primary_10_1107_S1600577522007019 crossref_primary_10_1107_S1600577524012141 crossref_primary_10_1016_j_jnucmat_2023_154743 |
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| Copyright | 2022 Alexander Scott Ditter et al. published by IUCr Journals. open access. 2022. This work is published under http://creativecommons.org/licenses/by/4.0/ (the "License"). Notwithstanding the ProQuest Terms and Conditions, you may use this content in accordance with the terms of the License. Alexander Scott Ditter et al. 2022 2022 |
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| Snippet | Soft X‐ray spectromicroscopy at the O K‐edge, U N4,5‐edges and Ce M4,5‐edges has been performed on focused ion beam sections of spent nuclear fuel for the... Soft X-ray spectromicroscopy at the O K -edge, U N 4,5 -edges and Ce M 4,5 -edges has been performed on focused ion beam sections of spent nuclear fuel for the... Soft X-ray spectromicroscopy at the O K-edge, U N -edges and Ce M -edges has been performed on focused ion beam sections of spent nuclear fuel for the first... Soft X-ray spectromicroscopy at the O K-edge, U N4,5-edges and Ce M4,5-edges has been performed on focused ion beam sections of spent nuclear fuel for the... |
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| SubjectTerms | Actinide Physics and Chemistry Atom probe analysis Bulk sampling Fission products focused ion beam sections INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND TECHNOLOGY Ion beams Microscopy NUCLEAR FUEL CYCLE AND FUEL MATERIALS Nuclear fuels Oxidation oxygen K-edge Radioactive wastes Spectroscopy spent nuclear fuel Spent nuclear fuels STCM STXM Uranium Uranium dioxide Uranium oxides Valence |
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| Title | Chemical and elemental mapping of spent nuclear fuel sections by soft X‐ray spectromicroscopy |
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