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Numerous metallurgical and materials science applications depend onquantitative atomic-scale characterizations of environmentally-sensitivematerials and their transient states. Studying the effect upon materialssubjected to thermochemical treatments in specific gaseous atmospheres is ofcentral importance for specifically studying a material's resistance to certainoxidative or hydrogen environments. It is also important for investigatingcatalytic materials, direct reduction of an oxide, particular surface sciencereactions or nanoparticle fabrication routes. This manuscript realizes suchexperiments upon a thermochemical reaction chamber called the Reacthub andallows for transferring treated materials under cryogenic & ultrahigh vacuumworkflow conditions for characterisation by either atom probe or scanningXe+/electron microscopies. Two examples are discussed in the present study. Oneprotocol was in the deuterium gas charging (25 kPa D2 at 200 {\deg}C) of ahigh-manganese twinning-induced-plasticity steel and characterization of theingress and trapping of hydrogen at various features (grain boundaries inparticular) in efforts to relate this to the steel's hydrogen embrittlementsusceptibility. Deuterium was successfully detected after gas charging but mostcontrast originated from the complex ion FeOD+ signal and the feature may be anartefact. The second example considered the direct deuterium reduction (5 kPaD2 at 700 {\deg}C) of a single crystal wuestite sample, demonstrating thatunder a standard thermochemical treatment causes rapid reduction upon thenanoscale. Further studies are required for complete confidence about thesephenomena, but these experiments successfully demonstrate that how an ex-situthermochemical treatment can be realised that capturesenvironmentally-sensitive transient states that can be analysed by atomic-scaleby atom probe microscope.

Laser-equipped gas reaction chamber for probing environmentally sensitive materials at near atomic scale