Abstract
We present sample transfer instrumentation and integrated protocols for the preparation and atom probe characterization of environmentally-sensitive materials. Ultra-high vacuum cryogenic suitcases allow specimen transfer between preparation, processing and several imaging platforms without exposure to atmospheric contamination. For expedient transfers, we installed a fast-docking station equipped with a cryogenic pump upon three systems; two atom probes, a scanning electron microscope / Xe-plasma focused ion beam and a N2-atmosphere glovebox. We also installed a plasma FIB with a solid-state cooling stage to reduce beam damage and contamination, through reducing chemical activity and with the cryogenic components as passive cryogenic traps. We demonstrate the efficacy of the new laboratory protocols by the successful preparation and transfer of two highly contamination- and temperature-sensitive samples—water and ice. Analysing pure magnesium atom probe data, we show that surface oxidation can be effectively suppressed using an entirely cryogenic protocol (during specimen preparation and during transfer). Starting with the cryogenically-cooled plasma FIB, we also prepared and transferred frozen ice samples while avoiding significant melting or sublimation, suggesting that we may be able to measure the nanostructure of other normally-liquid or soft materials. Isolated cryogenic protocols within the N2 glove box demonstrate the absence of ice condensation suggesting that environmental control can commence from fabrication until atom probe analysis.
Highlights
Atom probe tomography (APT) is an essential analytical tool for advancing modern material science applied to engineering materials [1], the life sciences [2] and geology [3]
Pure magnesium samples were prepared in the Helios plasma focusedion beam (PFIB) using an in-built micromanipulator and Pt-precursor gas injection system (GIS) to provide standard liftout techniques to mount samples upon a silicon microtip array
Each sample was transferred via the Ultra-high vacuum carry transfer suitcase (UHVCTS) to the LEAP 5000XR using with slightly different protocols
Summary
Atom probe tomography (APT) is an essential analytical tool for advancing modern material science applied to engineering materials [1], the life sciences [2] and geology [3]. Cryogenic UHV protocols for preparing and transferring atom probe samples no role in study design, data collection and analysis, decision to publish, or preparation of the manuscript
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