2018/05/28 by Leigh T. Stephenson, Agnieszka Szczepaniak, Stephenson, Leigh T. +29
Engineering · Materials Science · #Advanced Materials Characterization Techniques #FOS: Physical sciences #Hydrogen embrittlement and corrosion behaviors in metals #Materials Science (cond-mat.mtrl-sci) #Metal and Thin Film Mechanics
paper · pdf · doi:10.48550/arxiv.1805.10836
openalex publication_date 2018/05/28 · openalex created_date 2018/06/01 · openalex updated_date 2026/07/28
We present sample transfer instrumentation and integrated protocols for the preparation and correlative characterization of environmentally-sensitive materials by both atom probe tomography and electron microscopy. 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.