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

Schreiber, D. K.; Perea, D. E.; Ryan, J. V.; Evans, J. E.; Vienna, J. D.

doi:10.1016/J.ULTRAMIC.2018.07.010

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

Journal Article · Wed Jul 25 00:00:00 EDT 2018 · Ultramicroscopy

DOI:https://doi.org/10.1016/J.ULTRAMIC.2018.07.010· OSTI ID:1463336

^[1]; ^[2]; Ryan, J. V. ^[1]; Evans, J. E. ^[2]; Vienna, J. D. ^[1]

Pacific Northwest National Lab. (PNNL), Richland, WA (United States). Energy and Environment Directorate
Pacific Northwest National Lab. (PNNL), Richland, WA (United States). Earth and Biological Sciences Directorate

In this paper, 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. Finally, persistent challenges are discussed in addition to future opportunities for this new specimen preparation method.

View Accepted Manuscript (DOE)

Research Organization:: Energy Frontier Research Centers (EFRC) (United States). Center for Performance and Design of Nuclear Waste Forms and Containers (WastePD); Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22); USDOE Office of Science (SC), Biological and Environmental Research (BER) (SC-23)

Grant/Contract Number:: AC05-76RL01830; SC0016584

OSTI ID:: 1463336

Alternate ID(s):: OSTI ID: 1600933
OSTI ID: 1692161
OSTI ID: 23117987
OSTI ID: 1490238

Report Number(s):: PNNL-SA--133479; PII: S0304399118301153

Journal Information:: Ultramicroscopy, Journal Name: Ultramicroscopy Vol. 194; ISSN 0304-3991

Publisher:: ElsevierCopyright Statement

Country of Publication:: United States

Language:: English

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Ti and its alloys as examples of cryogenic focused ion beam milling of environmentally-sensitive materials Chang, Yanhong; Lu, Wenjun; Guénolé, Julien RWTH Aachen University https://doi.org/10.18154/rwth-2019-02232	text	January 2019
Atom Probe Tomography for 3D Structural and Chemical Analysis of Individual Proteins Sundell, Gustav; Hulander, Mats; Pihl, Astrid Small, Vol. 15, Issue 24 https://doi.org/10.1002/smll.201900316	journal	May 2019
Ti and its alloys as examples of cryogenic focused ion beam milling of environmentally-sensitive materials Chang, Yanhong; Lu, Wenjun; Guénolé, Julien Nature Communications, Vol. 10, Issue 1 https://doi.org/10.1038/s41467-019-08752-7	journal	February 2019
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Cryogenic specimens for nanoscale characterization of solid–liquid interfaces Zachman, Michael J.; de Jonge, Niels; Fischer, Robert MRS Bulletin, Vol. 44, Issue 12 https://doi.org/10.1557/mrs.2019.289	journal	December 2019
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47 OTHER INSTRUMENTATION
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A method for site-specific and cryogenic specimen fabrication of liquid/solid interfaces for atom probe tomography

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References (37)

Cited By (6)

Figures / Tables (9)

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