The Laplace Project: an integrated suite for preparing and transferring atom probe samples under cryogenic and UHV conditions

Autor: Agnieszka Szczepaniak, Isabelle Mouton, Jeffrey D. Shepard, Andreas Sturm, Yanhong Chang, Dierk Raabe, Uwe Tezins, Leigh T. Stephenson, Urs Maier, Andrew J. Breen, Thomas F. Kelly, Paraskevas Kontis, Dirk Vogel, Alex Rosenthal, Baptiste Gault, Kristiane A. K. Rusitzka
Jazyk: angličtina
Rok vydání: 2018
Předmět:
Scanning electron microscope
Glaciology
Condensation
02 engineering and technology
Atom probe
01 natural sciences
Focused ion beam
law.invention
law
Ice Cores
Electron Microscopy
Tomography
010302 applied physics
Microscopy
Multidisciplinary
Physics
Liquid Nitrogen
Chemical Reactions
Cryopump
021001 nanoscience & nanotechnology
Condensed Matter Physics
Cold Temperature
Chemistry
Glovebox
Physical Sciences
Optoelectronics
Medicine
Scanning Electron Microscopy
0210 nano-technology
Phase Transitions
Research Article
Chemical Elements
Fabrication
Materials science
Vacuum
Nitrogen
Science
Materials Science
Research and Analysis Methods
0103 physical sciences
Oxidation
business.industry
Ice
Water
Liquid nitrogen
Nanostructures
Oxygen
Specimen Preparation and Treatment
Earth Sciences
Sublimation (phase transition)
business
Hydrogen
Zdroj: PLoS ONE
PLoS One
PLoS ONE, Vol 13, Iss 12, p e0209211 (2018)
Popis: 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.
Databáze: OpenAIRE
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