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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: martin.meier@materials.ox.ac.uk
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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
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Copyright
Copyright © The Author(s), 2021. Published by Cambridge University Press on behalf of the Microscopy Society of America

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