Extending Estimating Hydrogen Content in Atom Probe Tomography Experiments Where H2 Molecule Formation Occurs

Meier, Markus; Jones, Megan E.; Felfer, Peter; Moody, Michael P.; Haley, Daniel

doi:10.1017/s1431927621012332

Cited by 17 publications

(4 citation statements)

References 26 publications

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“…Charging deuterium into APT specimens allows the distinction of experimentally introduced signals from the hydrogen background noise arising from the residual gas in the APT chamber [15] . While some studies have shown that using hydrogen charging can also provide qualitative measurements of hydrogen trapping [74] , deuterium charging has been demonstrated to reduce ambiguity in observations [15] . Furthermore, deuterium charging must be combined with voltage-pulsed APT, as laser-pulsed APT can produce a significant amount of 1 H 2 + peak at 2 m/z, leading to confusion when assigning 2 m/z to deuterium ( 2 H + ) [75] .…”

Section: Hydrogen In Metals and Alloysmentioning

confidence: 99%

Cryogenic atom probe tomography and its applications: a review

Zhou,

Wang,

Niu

et al. 2023

Microstructures

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Cryogenic atom probe tomography (cryo-APT) is a new microstructure characterization technique with the potential to address challenges across various research fields. In this review, we provide an overview of the development of cryo-APT and the associated instrumentation that transforms conventional APT into cryo-APT. We start by introducing the APT principle and the instrumentation involved in the cryo-APT workflow, emphasizing the key techniques that enable cryo-APT specimen preparation. Furthermore, we shed light on the research made possible by cryo-APT, presenting several recent outcomes to demonstrate its capabilities effectively. Finally, we discuss the limitations of cryo-APT and summarize the potential research areas that can further benefit from this cutting-edge microstructural characterization technique.

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Section: Hydrogen In Metals and Alloysmentioning

confidence: 99%

Cryogenic atom probe tomography and its applications: a review

Zhou,

Wang,

Niu

et al. 2023

Microstructures

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“…The deuterium, providing a peak in the mass spectrum at 2 Da, can therefore be clearly distinguished from hydrogen in the chamber, which has a peak at 1 Da, in voltage measurements. Charging can be done by means of electrolytic charging (Barton et al, 2024;Chen et al, 2017;Haley et al, 2014) or gas phase charging (Chen et al, 2017(Chen et al, , 2019(Chen et al, , 2020Haley et al, 2017Haley et al, , 2019Ishikawa & Yoshimura, 1998;Kesten et al, 2002;Khanchandani et al, 2021Khanchandani et al, , 2022Meier et al, 2022;Takahashi et al, 2010Takahashi et al, , 2012Takahashi et al, , 2018Takahashi et al, , 2021, whereby the latter generates less contamination and is therefore preferred (Khanchandani et al, 2021). This has often been the main solution in the past.…”

Section: Introductionmentioning

confidence: 99%

Miniaturized gas exposure devices for atom probe experiments

Ott,

Heller,

Monajem

et al. 2024

Microscopy Res & Technique

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To detect hydrogen in materials at the atomic scale, atom probe tomography is now regularly used. In order to avoid cumbersome cryo‐preparation to suppress diffusion, often hydrogen is charged only into the finished specimen. Here, the use of hydrogen gas over electrochemical hydrogen has the advantage that the specimen is not contaminated with an electrolyte. So far, this “charging” has been done in large, expensive systems. Here, we introduce small devices that enable the exposure of atom probe specimens to hydrogen and potentially other gases, using only very small gas volumes. This enables the operation in regular laboratory environments without additional safety measures. These devices can be used to expose the specimen to hydrogen up to 10 bar/90°C. Higher temperatures may be attained with small changes. Validation of the success of charging with these setups is demonstrated through experiments employing deuterium charging of palladium atom probe tips.Research Highlights Enabling the exposure of atom probe specimens to hydrogen and potentially other gases, using only very small gas volumes. Built setups can be assembled with little money and from freely available parts, making specimen charging much easier. Validation of the success of charging with these setups is demonstrated through experiments employing deuterium charging of palladium atom probe tips.

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“…The beauty of APT lies in the ability of detecting all elements with equal sensitivity at once, as it is based on the time-of-flight principle. Fine-scale 3D mapping of hydrogen in real space [9,10] is highly motivated by, e.g., studies of hydrogen embrittlement in metallic materials [11][12][13] and the impact of hydrogen in semiconductors [14][15][16]. APT is also used for developing hydrogen storage materials and their potential applications in catalytic reactions such as CO 2 methanation [17].…”

Section: Introductionmentioning

confidence: 99%

Deuterium Distribution in Fe/V Multi-Layered Films

2022

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The recent progress of Atom Probe Tomography (APT) has opened up atomic-scale elemental analysis including hydrogen species. For APT measurements, the use of deuterium is highly recommended, due to its low mobility compared to the fast and quantum mechanically tunneling isotope hydrogen. In addition, deuterium can be distinguished from hydrogen originating from the APT analysis chamber. To date, however, APT studies on materials with high D concentrations are scarce. In this study, the D concentration profile in a Fe/V multi-layered film sample was investigated, and spanned a wide concentration range. The mean hydrogen isotope concentration was alternatively quantified by electromotive force (EMF) measurements on a similar Fe/V film, thus verifying the APT results. The reduction found in the D concentration at the Fe/V interface results from local alloying at the Fe/V interfaces which accompanies a change in the available volume in the V lattice. Even at the same Fe concentration, the shape of the observed D depth profile was asymmetric at high D2 pressures. This indicates a stress impact caused by the deposition sequence.

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Extending Estimating Hydrogen Content in Atom Probe Tomography Experiments Where H2 Molecule Formation Occurs

Abstract: Abstract

Cited by 17 publications

References 26 publications

Cryogenic atom probe tomography and its applications: a review

Cryogenic atom probe tomography and its applications: a review

Miniaturized gas exposure devices for atom probe experiments

Deuterium Distribution in Fe/V Multi-Layered Films

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