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Ultramicroscopy. 2018 Nov;194:89-99. doi: 10.1016/j.ultramic.2018.07.010. Epub 2018 Jul 25.

A method for site-specific and cryogenic specimen fabrication of liquid/solid interfaces for atom probe tomography.

Author information

1
Energy and Environment Directorate, Pacific Northwest National Laboratory, P.O. Box 999, Richland, WA 99352, USA. Electronic address: daniel.schreiber@pnnl.gov.
2
Earth and Biological Sciences Directorate, Pacific Northwest National Laboratory, P.O. Box 999 Richland, WA 99352, USA. Electronic address: daniel.perea@pnnl.gov.
3
Energy and Environment Directorate, Pacific Northwest National Laboratory, P.O. Box 999, Richland, WA 99352, USA.
4
Earth and Biological Sciences Directorate, Pacific Northwest National Laboratory, P.O. Box 999 Richland, WA 99352, USA.

Abstract

A site-specific, cryogenic, focused ion beam (FIB) method is presented for the preparation of atom probe tomography (APT) specimens from a frozen liquid/solid interface. As a practical example, the interface between water and a corroded boroaluminosilicate glass has been characterized by APT for the first time. The water/glass interface is preserved throughout specimen preparation by plunge freezing the corroding glass particles with the corrosion solution into slush nitrogen. Site-specific specimen preparation is enabled through a new approach to extract and mount a small volume of material using a cryogenically cooled FIB stage and micromanipulator. The prepared APT specimens are subsequently transferred from the FIB to APT under cryogenic and high-vacuum conditions using a novel FIB/APT transfer shuttle and home-built environmental transfer hub attached to the APT system. Particular focus is given to the technical methods for specimen fabrication under cryogenic conditions. Persistent challenges are discussed in addition to future opportunities for this new specimen preparation method.

KEYWORDS:

Atom probe tomography; Corrosion; Cryogenic; Focused ion beam; Glass; Liquid/solid interfaces; Site-specific

PMID:
30092393
DOI:
10.1016/j.ultramic.2018.07.010
[Indexed for MEDLINE]

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