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Title: Site specific, high-resolution characterisation of porosity in graphite using FIB-SEM tomography

Abstract

Graphite is used as a moderator of fast neutrons in some types of nuclear reactors and for other industrial applications. The influence of smaller pores on the mechanical and physical properties of graphite remains to be fully understood. Here in this work, focused ion beam-scanning electron microscopy (FIB-SEM) tomography was applied to characterise the porosity of AGX graphite – an electrode material. FIB-SEM tomography consists in alternating the ion milling and SEM imaging at an area of interest with the objective of creating a 3D reconstruction. Regions containing a filler and a mixture of filler and binder were selected as the areas of interest. Resolutions of a few nanometers were achieved in volumes up to 1400 μm 3 for both regions. Typical porous structures were detected in the filler and binder regions such as thermal cracks, gas evolution porosity and lenticular pores. The resolution achieved with these experiments made possible detection of pores smaller than 150 nm in diameter, that is of the length scale of voids generated by neutron irradiation, and an improvement in spatial resolution of traditional x-ray tomography studies. The resolution achieved by FIB-SEM tomography may be essential for the study of the microstructure of graphite, providingmore » complimentary data to x-ray tomography experiments.« less

Authors:
ORCiD logo [1]; ORCiD logo [1]; ORCiD logo [1]; ORCiD logo [1]
  1. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Publication Date:
Research Org.:
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
1471932
Grant/Contract Number:  
AC05-00OR22725
Resource Type:
Journal Article: Accepted Manuscript
Journal Name:
Journal of Nuclear Materials
Additional Journal Information:
Journal Volume: 511; Journal Issue: C; Journal ID: ISSN 0022-3115
Publisher:
Elsevier
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE

Citation Formats

Arregui-Mena, Jose' D., Edmondson, Philip D., Campbell, Anne A., and Katoh, Yutai. Site specific, high-resolution characterisation of porosity in graphite using FIB-SEM tomography. United States: N. p., 2018. Web. doi:10.1016/j.jnucmat.2018.08.047.
Arregui-Mena, Jose' D., Edmondson, Philip D., Campbell, Anne A., & Katoh, Yutai. Site specific, high-resolution characterisation of porosity in graphite using FIB-SEM tomography. United States. doi:10.1016/j.jnucmat.2018.08.047.
Arregui-Mena, Jose' D., Edmondson, Philip D., Campbell, Anne A., and Katoh, Yutai. Sat . "Site specific, high-resolution characterisation of porosity in graphite using FIB-SEM tomography". United States. doi:10.1016/j.jnucmat.2018.08.047.
@article{osti_1471932,
title = {Site specific, high-resolution characterisation of porosity in graphite using FIB-SEM tomography},
author = {Arregui-Mena, Jose' D. and Edmondson, Philip D. and Campbell, Anne A. and Katoh, Yutai},
abstractNote = {Graphite is used as a moderator of fast neutrons in some types of nuclear reactors and for other industrial applications. The influence of smaller pores on the mechanical and physical properties of graphite remains to be fully understood. Here in this work, focused ion beam-scanning electron microscopy (FIB-SEM) tomography was applied to characterise the porosity of AGX graphite – an electrode material. FIB-SEM tomography consists in alternating the ion milling and SEM imaging at an area of interest with the objective of creating a 3D reconstruction. Regions containing a filler and a mixture of filler and binder were selected as the areas of interest. Resolutions of a few nanometers were achieved in volumes up to 1400 μm3 for both regions. Typical porous structures were detected in the filler and binder regions such as thermal cracks, gas evolution porosity and lenticular pores. The resolution achieved with these experiments made possible detection of pores smaller than 150 nm in diameter, that is of the length scale of voids generated by neutron irradiation, and an improvement in spatial resolution of traditional x-ray tomography studies. The resolution achieved by FIB-SEM tomography may be essential for the study of the microstructure of graphite, providing complimentary data to x-ray tomography experiments.},
doi = {10.1016/j.jnucmat.2018.08.047},
journal = {Journal of Nuclear Materials},
number = C,
volume = 511,
place = {United States},
year = {Sat Dec 01 00:00:00 EST 2018},
month = {Sat Dec 01 00:00:00 EST 2018}
}

Journal Article:
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