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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 [1]; ORCiD logo [2];  [1];  [2];  [1]
  1. Pacific Northwest National Lab. (PNNL), Richland, WA (United States). Energy and Environment Directorate
  2. Pacific Northwest National Lab. (PNNL), Richland, WA (United States). Earth and Biological Sciences Directorate
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); The Ohio State Univ., Columbus, OH (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES); USDOE Office of Science (SC), Biological and Environmental Research (BER)
OSTI Identifier:
1463336
Alternate Identifier(s):
OSTI ID: 1600933; OSTI ID: 1692161
Report Number(s):
PNNL-SA-133479
Journal ID: ISSN 0304-3991; PII: S0304399118301153
Grant/Contract Number:  
AC05-76RL01830; SC0016584; 66382
Resource Type:
Accepted Manuscript
Journal Name:
Ultramicroscopy
Additional Journal Information:
Journal Volume: 194; Journal ID: ISSN 0304-3991
Publisher:
Elsevier
Country of Publication:
United States
Language:
English
Subject:
47 OTHER INSTRUMENTATION; atom probe tomography; focused ion beam; cryogenic; site-specific; corrosion; liquid/solid interfaces; glass; 36 MATERIALS SCIENCE; Site specific; Liquid solid interfaces

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. https://doi.org/10.1016/J.ULTRAMIC.2018.07.010
Schreiber, D. K., Perea, D. E., Ryan, J. V., Evans, J. E., and Vienna, J. D. Wed . "A method for site-specific and cryogenic specimen fabrication of liquid/solid interfaces for atom probe tomography". United States. https://doi.org/10.1016/J.ULTRAMIC.2018.07.010. https://www.osti.gov/servlets/purl/1463336.
@article{osti_1463336,
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},
number = ,
volume = 194,
place = {United States},
year = {2018},
month = {7}
}

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Figures / Tables:

Figure 1 Figure 1: Optical photographs of the sample loading procedure prior to plunge freezing. (a) A modified APT puck is loaded with a standard Cu spring clip and Si micropost array. A small droplet of water containing corroded glass powder is dropcast directly onto the spring clip. (b) The puck ismore » attached to the shuttle carrier end effector (puckulator) prior to plunge freezing and direct loading into the cryogenic FIB loadlock system. (c) LEAP buffer chamber carousel with a modified APT specimen puck slot made from thermally insulating Techtron® PPS material.« less

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