Analysis of deuterium in V–Fe5at.% film by atom probe tomography (APT)

Gemma, Ryota; Al-Kassab, T.; Kirchheim, R.; Pundt, Astrid

doi:10.1016/j.jallcom.2010.11.122

Cited by 26 publications

(36 citation statements)

References 28 publications

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“…Nevertheless, this is exactly the procedure necessary for correlating micro-structural features and their activity for hydrogen release, contrary to other techniques that just allow the measurement of the presence of hydrogen at a certain site, such as e.g tritium autoradiography or microcontact printing. Even recent successes of using atom probes for measuring hydrogen at trap sites, with atomic and elemental resolution [87, 88] will not readily provide information on the release activity of these trap sites, as it is a destructive method only providing snapshots, although of extreme resolution.…”

Section: The New Method: Hydrogen Detection By a Kelvin Probementioning

confidence: 99%

Hydrogen detection in metals: a review and introduction of a Kelvin probe approach

Evers

Şenöz

Rohwerder

2013

Science and Technology of Advanced Materials

113

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Hydrogen in materials is an important topic for many research fields in materials science. Hence in the past quite a number of different techniques for determining the amount of hydrogen in materials and for measuring hydrogen permeation through them have been developed. Some of these methods have found widespread application. But for many problems the achievable sensitivity is usually not high enough and ready-to-use techniques providing also good spatial resolution, especially in the submicron range, are very limited, and mostly not suitable for widespread application. In this work this situation will be briefly reviewed and a novel scanning probe technique based method introduced.

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Section: The New Method: Hydrogen Detection By a Kelvin Probementioning

confidence: 99%

Hydrogen detection in metals: a review and introduction of a Kelvin probe approach

Evers

Şenöz

Rohwerder

2013

Science and Technology of Advanced Materials

113

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“…Results on H/D analysis using APT for solutes and stable hydrides remain limited but reports can be found in the literature for multilayered materials [13,19], Ti-based [20][21][22][23] or Zr-based alloys [24] for instance. Deuteration is however not without challenges since H can be detected both as atomic ions, i.e.…”

Section: Introductionmentioning

confidence: 99%

Solute hydrogen and deuterium observed at the near atomic scale in high-strength steel

et al. 2020

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Observing solute hydrogen (H) in matter is a formidable challenge, yet, enabling quantitative imaging of H at the atomic-scale is critical to understand its deleterious influence on the mechanical strength of many metallic alloys that has resulted in many catastrophic failures of engineering parts and structures. Here, we report on the APT analysis of hydrogen (H) and deuterium (D) within the nanostructure of an ultra-high strength steel with high resistance to hydrogen embrittlement. Cold drawn, severely deformed pearlitic steel wires (Fe-0.98C-0.31Mn-0.20Si-0.20Cr-0.01Cu-0.006P-0.007S wt.%, = 3.1) contains cementite decomposed during the pre-deformation of the alloy and ferrite. We find H and D within the decomposed cementite, and at some interfaces with the surrounding ferrite. To ascertain the origin of the H/D signal obtained in APT, we explored a series of experimental workflows including cryogenic specimen preparation and cryogenic-vacuum transfer from the preparation into a state-of-the-art atom probe. Our study points to the critical role of the preparation, i.e. the possible saturation of H-trapping sites during electrochemical polishing, how these can be alleviated by the use of an outgassing treatment, cryogenic preparation and transfer prior to charging. Accommodation of large amounts of H in the under-stoichiometric carbide likely explains the resistance of pearlite against hydrogen embrittlement.

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“…In principle the "background" hydrogen challenge can be overcome with isotopic marking, using deuterium, as the natural abundance of deuterium is very low (only 0.015%). Isotopic marking, through the use of deuterium or heavy water during microstructural formation, has been used to distinguish between residual hydrogen from the chamber and solute hydrogen, the deuterium, originating from the specimen itself (Gemma et al, 2007(Gemma et al, , 2011Takahashi et al, 2010Takahashi et al, , 2018Chen et al, 2017;Li et al, 2018).…”

Section: Introductionmentioning

confidence: 99%

Quantification Challenges for Atom Probe Tomography of Hydrogen and Deuterium in Zircaloy-4

et al. 2019

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Analysis and understanding of the role of hydrogen in metals is a significant challenge for the future of materials science, and this is a clear objective of recent work in the atom probe tomography (APT) community. Isotopic marking by deuteration has often been proposed as the preferred route to enable quantification of hydrogen by APT. Zircaloy-4 was charged electrochemically with hydrogen and deuterium under the same conditions to form large hydrides and deuterides. Our results from a Zr hydride and a Zr deuteride highlight challenges associated to accurate quantification of hydrogen and deuterium, in particular associated to the overlap of peaks at low mass-to-charge ratio and of hydrogen/deuterium containing molecular ions. We discuss possible ways to ensure that appropriate information is extracted from APT analysis of hydrogen in a zirconium alloy systems that is important for nuclear power.

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Analysis of deuterium in V–Fe5at.% film by atom probe tomography (APT)

Cited by 26 publications

References 28 publications

Hydrogen detection in metals: a review and introduction of a Kelvin probe approach

Hydrogen detection in metals: a review and introduction of a Kelvin probe approach

Solute hydrogen and deuterium observed at the near atomic scale in high-strength steel

Quantification Challenges for Atom Probe Tomography of Hydrogen and Deuterium in Zircaloy-4

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