Atom Probe Analysis of Ex Situ Gas-Charged Stable Hydrides 313
oxygen for rapidly oxidizing samples is a key requirement. For more inert materials, ex situ D charging can correctly identify D atoms within the metallic matrix readily, and is a feasible route for hydride analysis. There remain several concerns for estimating the
quantity of deuterium within the samples. Further work needs to be undertaken in order to fully understand the geometrical effect that arises from the use of needle samples, to which the reduced D content within these hydrides is attributed. Comparisons can be drawn with existing litera- ture on hydrided samples, such as Nb measured by ERD (Maheshwari et al., 2011; Romanenko & Goncharova, 2011).
CONCLUSIONS
In this work, we have demonstrated the capability of atom probe to performex situ hydriding studies of bulk hydrides, in the form of Pd–Rh-D. Within this material, a clear, spatially discriminated signal is observable on timescales that are, despite the small length scales inherent in APT, amenable to atom probe analysis. The stability of these hydrides was shown to be sufficient to allow for regular experimentation. However, there remains a discrepancy between the equilibrium solubilities that should be identifiable within this material, and the quantitative concentrations that have been observedwithin this work. For materials that rapidly form native oxides, it has been shown that the oxide layer itself may contain small quantities of deuterium, however an in situ approach may be a more feasible alternative (Dumpala et al., 2015), depending upon the propensity for the surface to oxidize. Further work in this area should expand the pressure/temperature space that is experimentally available to atomprobe, as well as to undertake multi-technique analyses, to fully understand the quantitative capacity of atom probe in deuterated studies.
ACKNOWLEDGMENTS
The authors acknowledge the support of the EPSRC under the HEmS Programme Grant EP/L014742/1.
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