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

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.

Authors:
ORCiD logo; ORCiD logo; ; ;
Publication Date:
Research Org.:
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 Org.:
USDOE
OSTI Identifier:
1490238
Report Number(s):
PNNL-SA-133479
Journal ID: ISSN 0304-3991
DOE Contract Number:  
AC05-76RL01830
Resource Type:
Journal Article
Journal Name:
Ultramicroscopy
Additional Journal Information:
Journal Volume: 194; Journal Issue: C; Journal ID: ISSN 0304-3991
Publisher:
Elsevier
Country of Publication:
United States
Language:
English
Subject:
cryogenic FIB, atom probe tomography (APT), corrosion, glass

Citation Formats

Schreiber, D. K., Perea, D. E., Ryan, J. V., Evans, J. E., and Vienna, J. D. A method for site-specific and cryogenic specimen fabrication of liquid/solid interfaces for atom probe tomography. United States: N. p., 2018. Web. doi:10.1016/j.ultramic.2018.07.010.
Schreiber, D. K., Perea, D. E., Ryan, J. V., Evans, J. E., & Vienna, J. D. A method for site-specific and cryogenic specimen fabrication of liquid/solid interfaces for atom probe tomography. United States. doi:10.1016/j.ultramic.2018.07.010.
Schreiber, D. K., Perea, D. E., Ryan, J. V., Evans, J. E., and Vienna, J. D. Thu . "A method for site-specific and cryogenic specimen fabrication of liquid/solid interfaces for atom probe tomography". United States. doi:10.1016/j.ultramic.2018.07.010.
@article{osti_1490238,
title = {A method for site-specific and cryogenic specimen fabrication of liquid/solid interfaces for atom probe tomography},
author = {Schreiber, D. K. and Perea, D. E. and Ryan, J. V. and Evans, J. E. and Vienna, J. D.},
abstractNote = {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.},
doi = {10.1016/j.ultramic.2018.07.010},
journal = {Ultramicroscopy},
issn = {0304-3991},
number = C,
volume = 194,
place = {United States},
year = {2018},
month = {11}
}