Abstract
To detect hydrogen in materials at the atomic scale, atom probe
tomography is now regularly used. In order to avoid cumbersome
cryo-preparation to suppress diffusion, often hydrogen is charged only
into the finished specimen. Here, the use of hydrogen gas over
electrochemical hydrogen has the advantage that the specimen is not
contaminated with an electrolyte. So far, this ‘charging’ has been done
in large, expensive systems. Here, we introduce small devices that
enable the exposure of atom probe specimens to hydrogen and potentially
other gases, using only very small gas volumes. This enables the
operation in regular laboratory environments without additional safety
measures. These devices can be used to expose the specimen to hydrogen
up to 10 bar / 90 °C. Higher temperatures may be attained with small
changes. Validation of the success of charging with these setups is
demonstrated through experiments employing deuterium charging of
palladium atom probe tips.