期刊
MICROSCOPY AND MICROANALYSIS
卷 28, 期 4, 页码 1231-1244出版社
OXFORD UNIV PRESS
DOI: 10.1017/S1431927621012332
关键词
atom probe tomography; deuterium; evaporation rate; hydrogen; hydrogen peak height ratio; hydrogen/deuterium mass-to-charge spectrum overlap
资金
- Cameca Instruments
- EPSRC
- National Nuclear Laboratory
- EPSRC [EP/P001645/1]
- European Research Council (ERC) under the European Union [085065]
- Rolls Royce Plc.
This study investigated a new method for accurately estimating hydrogen content within specimen in atom probe tomography experiments. The research showed a highly correlated relationship between field evaporation rate and hydrogen content, leading to a new method for measuring hydrogen content. By combining extrapolation technique with continuous cycling of the evaporation rate during APT experiments, spatially resolved imaging of hydrogen concentrations could be achieved without the need for deuteration.
We investigated a new method for estimating specimen hydrogen content in atom probe tomography (APT) in experiments where molecular hydrogen ions (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 H+/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.
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