Quantification of solute deuterium in titanium deuteride by atom probe tomography with both laser pulsing and high-voltage pulsing: influence of the surface electric field
Atom probe tomography (APT) has been increasingly used to investigate hydrogen embrittlement in metals due to its unique capacity for direct imaging of H atoms interacting with microstructural features. The quantitativeness of hydrogen measurements by APT is yet to be established in views of erroneo...
| Main Authors: | , , , , , , , , , |
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| Format: | Article |
| Language: | English |
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IOP Publishing
2019-01-01
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| Series: | New Journal of Physics |
| Subjects: | |
| Online Access: | https://doi.org/10.1088/1367-2630/ab1c3b |
| _version_ | 1797750109518168064 |
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| author | Y H Chang I Mouton L Stephenson M Ashton G K Zhang A Szczpaniak W J Lu D Ponge D Raabe B Gault |
| author_facet | Y H Chang I Mouton L Stephenson M Ashton G K Zhang A Szczpaniak W J Lu D Ponge D Raabe B Gault |
| author_sort | Y H Chang |
| collection | DOAJ |
| description | Atom probe tomography (APT) has been increasingly used to investigate hydrogen embrittlement in metals due to its unique capacity for direct imaging of H atoms interacting with microstructural features. The quantitativeness of hydrogen measurements by APT is yet to be established in views of erroneous compositional measurements of bulk hydrides and the influence of spurious hydrogen, e.g. residual gas inside the analysis chamber. Here, we analyzed titanium deuteride (approx. 65.0 at%–66.6 at% D) in lieu of hydride to minimize the overlap with residual gas, both with laser pulsing and high-voltage (HV) pulsing. Strategies were deployed to prevent H pick-up during specimen fabrication, including preparing specimens at cryogenic temperature. The measured composition of deuterium by APT with laser pulsing decreases significantly with the applied laser pulse energy, which is interpreted with regards to the strength of the corresponding surface electrostatic field, as assessed by the evolution of charge-state ratio. In contrast, compositional analyses with HV pulsing are roughly independent of the applied experimental parameters, although approx. 15 at%–20 at% off the nominal composition. Aided by plotting paired mass-to-charge correlations, the mechanisms of composition bias in both pulsing modes are discussed. A special emphasis is placed on the local variations of the measured composition as a function of the local electric field across the specimen’s surface, which is not uniform due to asymmetric heat distribution related to the localized laser absorption and the faceted nature of surface caused by the crystallographic structure. Our investigations demonstrate the challenges of quantitative analysis of solute deuterium by APT but nevertheless provide insight to achieving the best possible experimental protocol. |
| first_indexed | 2024-03-12T16:28:54Z |
| format | Article |
| id | doaj.art-dee0d2268d9646128c04b44a2e296208 |
| institution | Directory Open Access Journal |
| issn | 1367-2630 |
| language | English |
| last_indexed | 2024-03-12T16:28:54Z |
| publishDate | 2019-01-01 |
| publisher | IOP Publishing |
| record_format | Article |
| series | New Journal of Physics |
| spelling | doaj.art-dee0d2268d9646128c04b44a2e2962082023-08-08T15:37:02ZengIOP PublishingNew Journal of Physics1367-26302019-01-0121505302510.1088/1367-2630/ab1c3bQuantification of solute deuterium in titanium deuteride by atom probe tomography with both laser pulsing and high-voltage pulsing: influence of the surface electric fieldY H Chang0I Mouton1L Stephenson2M Ashton3G K Zhang4A Szczpaniak5W J Lu6D Ponge7D Raabe8B Gault9Max Planck Institute für Eisenforschung GmbH , Düsseldorf, GermanyMax Planck Institute für Eisenforschung GmbH , Düsseldorf, Germany; CEA, DEN, Service de Recherches Métallurgiques Appliquées, Laboratoire d’Analyse Microstructurale des Matériaux, F-91191 Gif-sur-Yvette, FranceMax Planck Institute für Eisenforschung GmbH , Düsseldorf, GermanyMax Planck Institute für Eisenforschung GmbH , Düsseldorf, GermanyChina Academy of Engineering Physics, Institute of Materials , Jiangyou, People’s Republic of ChinaMax Planck Institute für Eisenforschung GmbH , Düsseldorf, GermanyMax Planck Institute für Eisenforschung GmbH , Düsseldorf, GermanyMax Planck Institute für Eisenforschung GmbH , Düsseldorf, GermanyMax Planck Institute für Eisenforschung GmbH , Düsseldorf, GermanyMax Planck Institute für Eisenforschung GmbH , Düsseldorf, Germany; Department of Materials, Royal School of Mines, Imperial College, Prince Consort Road, London, SW7 2BP, United KingdomAtom probe tomography (APT) has been increasingly used to investigate hydrogen embrittlement in metals due to its unique capacity for direct imaging of H atoms interacting with microstructural features. The quantitativeness of hydrogen measurements by APT is yet to be established in views of erroneous compositional measurements of bulk hydrides and the influence of spurious hydrogen, e.g. residual gas inside the analysis chamber. Here, we analyzed titanium deuteride (approx. 65.0 at%–66.6 at% D) in lieu of hydride to minimize the overlap with residual gas, both with laser pulsing and high-voltage (HV) pulsing. Strategies were deployed to prevent H pick-up during specimen fabrication, including preparing specimens at cryogenic temperature. The measured composition of deuterium by APT with laser pulsing decreases significantly with the applied laser pulse energy, which is interpreted with regards to the strength of the corresponding surface electrostatic field, as assessed by the evolution of charge-state ratio. In contrast, compositional analyses with HV pulsing are roughly independent of the applied experimental parameters, although approx. 15 at%–20 at% off the nominal composition. Aided by plotting paired mass-to-charge correlations, the mechanisms of composition bias in both pulsing modes are discussed. A special emphasis is placed on the local variations of the measured composition as a function of the local electric field across the specimen’s surface, which is not uniform due to asymmetric heat distribution related to the localized laser absorption and the faceted nature of surface caused by the crystallographic structure. Our investigations demonstrate the challenges of quantitative analysis of solute deuterium by APT but nevertheless provide insight to achieving the best possible experimental protocol.https://doi.org/10.1088/1367-2630/ab1c3batom probe tomographysurface electric fieldtitanium hydride/deuterideH/D quantification |
| spellingShingle | Y H Chang I Mouton L Stephenson M Ashton G K Zhang A Szczpaniak W J Lu D Ponge D Raabe B Gault Quantification of solute deuterium in titanium deuteride by atom probe tomography with both laser pulsing and high-voltage pulsing: influence of the surface electric field New Journal of Physics atom probe tomography surface electric field titanium hydride/deuteride H/D quantification |
| title | Quantification of solute deuterium in titanium deuteride by atom probe tomography with both laser pulsing and high-voltage pulsing: influence of the surface electric field |
| title_full | Quantification of solute deuterium in titanium deuteride by atom probe tomography with both laser pulsing and high-voltage pulsing: influence of the surface electric field |
| title_fullStr | Quantification of solute deuterium in titanium deuteride by atom probe tomography with both laser pulsing and high-voltage pulsing: influence of the surface electric field |
| title_full_unstemmed | Quantification of solute deuterium in titanium deuteride by atom probe tomography with both laser pulsing and high-voltage pulsing: influence of the surface electric field |
| title_short | Quantification of solute deuterium in titanium deuteride by atom probe tomography with both laser pulsing and high-voltage pulsing: influence of the surface electric field |
| title_sort | quantification of solute deuterium in titanium deuteride by atom probe tomography with both laser pulsing and high voltage pulsing influence of the surface electric field |
| topic | atom probe tomography surface electric field titanium hydride/deuteride H/D quantification |
| url | https://doi.org/10.1088/1367-2630/ab1c3b |
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