Hostname: page-component-78c5997874-ndw9j Total loading time: 0 Render date: 2024-11-02T19:12:09.014Z Has data issue: false hasContentIssue false
  • English
  • Français

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

Published online by Cambridge University Press:  28 July 2021

Martin S. Meier Open the ORCID record for Martin S. Meier [Opens in a new window] ,
Megan E. Jones Open the ORCID record for Megan E. Jones [Opens in a new window] ,
Peter J. Felfer ,
Michael P. Moody  and
Daniel Haley
Martin S. Meier*
Affiliation:
Department of Materials, University of Oxford, Parks Rd, Oxford, OX1 3PH, UK
Megan E. Jones
Affiliation:
Department of Materials, University of Oxford, Parks Rd, Oxford, OX1 3PH, UK
Peter J. Felfer
Affiliation:
Department of Materials Science and Engineering, Friedrich-Alexander-Universität Erlangen-Nürnberg, 91054 Erlangen, Germany
Michael P. Moody
Affiliation:
Department of Materials, University of Oxford, Parks Rd, Oxford, OX1 3PH, UK
Daniel Haley
Affiliation:
Department of Materials, University of Oxford, Parks Rd, Oxford, OX1 3PH, UK
*
*Corresponding author: Martin S. Meier, E-mail: [email protected]
Get access

Abstract

We investigated a new method for estimating specimen hydrogen content in atom probe tomography (APT) in experiments where molecular hydrogen ions (${\rm H}_2^ +$) originating from the measurement environment can overlap with deuterium (D+) in the mass-to-charge-state spectrum, thus preventing the direct application of isotopic marking for unambiguous hydrogen analysis. First, we applied an existing method for hydrogen content estimation, using ${\rm H}^ + {/}{\rm H}_2^ +$ ratios obtained from paired deuterated/nondeuterated experiments. These measurements demonstrated sufficient residual uncertainty to motivate exploring an alternative method to accurately estimate hydrogen content. By varying the time between evaporation events, it is then shown that a highly correlated relationship between field evaporation rate and hydrogen content exists and can also be used to predict hydrogen content. This leads to a new method for measuring hydrogen content within the specimen. We combine this extrapolation technique with continuous cycling of the evaporation rate or pulse frequency during an APT experiment. This could enable spatially resolved imaging of hydrogen concentrations despite the presence of a contaminant background hydrogen signal, without the need for deuteration.

Keywords

atom probe tomographydeuteriumevaporation ratehydrogenhydrogen peak height ratiohydrogen/deuterium mass-to-charge spectrum overlap
Type
Detection of Hydrogen
Information
Microscopy and Microanalysis , Volume 28 , Issue 4 , August 2022 , pp. 1231 - 1244
Check for updates
Copyright
Copyright © The Author(s), 2021. Published by Cambridge University Press on behalf of the Microscopy Society of America

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Al-Faqeer, FM, Weil, KG & Pickering, HW (2003). Analysis of hydrogen absorption under competitive adsorption conditions - Effect of hexamethylenetetramine. J Electrochem Soc 150(5), B211–B216.CrossRefGoogle Scholar
Breen, AJ, Stephenson, LT, Sun, B, Li, Y, Kasian, O, Raabe, D, Herbig, M & Gault, B (2020). Solute hydrogen and deuterium observed at the near atomic scale in high-strength steel. Acta Mater 188, 108–120.CrossRefGoogle Scholar
Chen, Y-S, Bagot, PAJ, Moody, MP & Haley, D (2019). Observing hydrogen in steel using cryogenic atom probe tomography: A simplified approach. Int J Hydrogen Energy 44(60), 32280–32291.CrossRefGoogle Scholar
Chen, Y-S, Haley, D, Gerstl, SSA, London, AJ, Sweeney, F, Wepf, RA, Rainforth, WM, Bagot, PAJ & Moody, MP (2017). Direct observation of individual hydrogen atoms at trapping sites in a ferritic steel. Science 355(6330), 1196–1199.CrossRefGoogle Scholar
Gemma, R, Al-Kassab, T, Kirchheim, R & Pundt, A (2009). APT analyses of deuterium-loaded Fe/V multi-layered films. Ultramicroscopy 109(5), 631–636.CrossRefGoogle ScholarPubMed
Haley, D, McCarroll, I, Bagot, PAJ, Cairney, JM & Moody, MP (2019). A Gas-phase reaction cell for modern atom probe systems. Microsc Microanal 25(2), 410–417.CrossRefGoogle ScholarPubMed
Haley, D, Merzlikin, SV, Choi, P & Raabe, D (2014). Atom probe tomography observation of hydrogen in high-Mn steel and silver charged via an electrolytic route. Int J Hydrogen Energy 39(23), 12221–12229.CrossRefGoogle Scholar
Jonathan Bennett & AutoIt Team (2018). AutoIt. Available at www.autoitscript.com (accessed June 12, 2019).Google Scholar
Kellogg, GL (1981). Pulsed laser stimulated field desorption of hydrogen from molybdenum. J Chem Phys 74(2), 1479–1487.CrossRefGoogle Scholar
Kellogg, GL & Panitz, JKG (1980). A direct observation of the trapping of deuterium ions at a grain boundary in tungsten. Appl Phys Lett 37(7), 625–627.CrossRefGoogle Scholar
Kellogg, GL & Tsong, TT (1980). Pulsed-laser atom-probe field-ion microscopy. J Appl Phys 51(2), 1184–1193.CrossRefGoogle Scholar
Kesten, P, Pundt, A, Schmitz, G, Weisheit, M, Krebs, HU & Kirchheim, R (2002). H- and D distribution in metallic multilayers studied by 3-dimensional atom probe analysis and secondary ion mass spectrometry. J Alloys Compd 330, 225–228.CrossRefGoogle Scholar
Kolli, RP (2017). Controlling residual hydrogen gas in mass spectra during pulsed laser atom probe tomography. Adv Struct Chem Imaging 3(1), 10.CrossRefGoogle ScholarPubMed
Krom, AHM & Bakker, A (2000). Hydrogen trapping models in steel. Metall Mater Trans B 31(6), 1475–1482.CrossRefGoogle Scholar
Liu, MA, Rivera-Díaz-del-Castillo, PEJ, Barraza-Fierro, JI, Castaneda, H & Srivastava, A (2019). Microstructural influence on hydrogen permeation and trapping in steels. Mater Des 167, 107605.CrossRefGoogle Scholar
London, AJ (2019). Quantifying uncertainty from mass-peak overlaps in atom probe microscopy. Microsc Microanal 25(2), 378–388.CrossRefGoogle ScholarPubMed
Marian, J, Hoang, T, Fluss, M & Hsiung, LL (2015). A review of helium–hydrogen synergistic effects in radiation damage observed in fusion energy steels and an interaction model to guide future understanding. J Nucl Mater 462, 409–421.CrossRefGoogle Scholar
Martin, TL, London, AJ, Jenkins, B, Hopkin, SE, Douglas, JO, Styman, PD, Bagot, PAJ & Moody, MP (2017). Comparing the consistency of atom probe tomography measurements of small-scale segregation and clustering between the LEAP 3000 and LEAP 5000 instruments. Microsc Microanal 23(2), 227–237.CrossRefGoogle ScholarPubMed
Prosa, TJ, Geiser, BP, Lawrence, D, Olson, D & Larson, DJ (2014). Developing detection efficiency standards for atom probe tomography. Proc. SPIE. 9173. https://doi.org/10.1117/12.2062211.CrossRefGoogle Scholar
Reddy, SM, Saxey, DW, Rickard, WDA, Fougerouse, D, Montalvo, SD, Verberne, R & van Riessen, A (2020). Atom probe tomography: Development and application to the geosciences. Geostand Geoanal Res 44(1), 5–50.CrossRefGoogle Scholar
Robertson, IM, Sofronis, P, Nagao, A, Martin, ML, Wang, S, Gross, DW & Nygren, KE (2015). Hydrogen embrittlement understood. Metall Mater Trans B 46(3), 1085–1103.CrossRefGoogle Scholar
Rusman, NAA & Dahari, M (2016). A review on the current progress of metal hydrides material for solid-state hydrogen storage applications. Int J Hydrogen Energy 41(28), 12108–12126.CrossRefGoogle Scholar
Sundell, G, Thuvander, M & Andren, HO (2013). Hydrogen analysis in APT: Methods to control adsorption and dissociation of H-2. Ultramicroscopy 132, 285–289.CrossRefGoogle Scholar
Takahashi, J, Kawakami, K & Kobayashi, Y (2018). Origin of hydrogen trapping site in vanadium carbide precipitation strengthening steel. Acta Mater 153, 193–204.CrossRefGoogle Scholar
Takahashi, J, Kawakami, K, Kobayashi, Y & Tarui, T (2010). The first direct observation of hydrogen trapping sites in TiC precipitation-hardening steel through atom probe tomography. Scr Mater 63(3), 261–264.CrossRefGoogle Scholar
Takahashi, J, Kawakami, K & Tarui, T (2012). Direct observation of hydrogen-trapping sites in vanadium carbide precipitation steel by atom probe tomography. Scr Mater 67(2), 213–216.CrossRefGoogle Scholar
Tsong, TT (1978). Measurement of the field evaporation rate of several transition metals. J Phys F Met Phys 8(7), 1349–1352.CrossRefGoogle Scholar
Supplementary material: PDF

Meier et al. supplementary material

Meier et al. supplementary material

Download Meier et al. supplementary material(PDF)
PDF 3.4 MB