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Atomprobe tomography (APT)has been increasingly used to investigate hydrogen embrittlement in metals due to its unique capacity for direct imaging ofH atoms interacting withmicrostructural features. The quantitativeness of hydrogenmeasurements byAPT is yet to be established in views of erroneous compositionalmeasurements of bulk hydrides and the influence of spurious hydrogen, e.g. residual gas inside the analysis chamber. Here, we analyzed titaniumdeuteride (approx. 65.0 at%–66.6 at%D) in lieu of hydride tominimize the overlapwith residual gas, bothwith laser pulsing and highvoltage (HV) pulsing. Strategies were deployed to preventHpick-up during specimen fabrication, including preparing specimens at cryogenic temperature. Themeasured composition of deuteriumby APTwith laser pulsing decreases significantly with the applied laser pulse energy, which is interpreted with regards to the strength of the corresponding surface electrostaticfield, as assessed by the evolution of charge-state ratio. In contrast, compositional analyses withHVpulsing are roughly independent of the applied experimental parameters, although approx. 15 at%–20 at%off the nominal composition. Aided by plotting pairedmass-to-charge correlations, themechanisms of composition bias in both pulsingmodes are discussed. A special emphasis is placed on the local variations of themeasured composition as a function of the local electricfield across the specimen’s surface, which is not uniform due to asymmetric heat distribution related to the localized laser absorption and the faceted nature of surface caused by the crystallographic structure.Our investigations demonstrate the challenges of quantitative analysis of solute deuteriumbyAPTbut nevertheless provide insight to achieving the best possible experimental protocol.

new journal of physics

Quantification of solute deuterium in titanium deuteride by atom probe tomography with both laser pulsing and high-voltage pulsing: influence of the surface electric field