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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 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 complimentarymore » 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
Alternate Identifier(s):
OSTI ID: 1635887
Grant/Contract Number:  
AC05-00OR22725
Resource Type:
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. https://doi.org/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. https://doi.org/10.1016/j.jnucmat.2018.08.047. https://www.osti.gov/servlets/purl/1471932.
@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 = {2018},
month = {12}
}

Works referenced in this record:

The microstructure of nuclear graphite binders
journal, January 2008


Microstructural characterization and pore structure analysis of nuclear graphite
journal, August 2011


Dimensional change, irradiation creep and thermal/mechanical property changes in nuclear graphite
journal, April 2016


Secondary ion mass spectrometric image depth profiling for three-dimensional elemental analysis
journal, January 1982

  • Patkin, Adam J.; Morrison, George H.
  • Analytical Chemistry, Vol. 54, Issue 1
  • DOI: 10.1021/ac00238a005

Subsurface nanoindentation deformation of Cu-Al multilayers mapped in 3D by focused ion beam microscopy
journal, February 2001


Three-dimensional analysis of porous BaTiO3 ceramics using FIB nanotomography
journal, October 2004


Overview of strength, crack propagation and fracture of nuclear reactor moderator graphite
journal, October 2013


Understanding fracture behaviour of PGA reactor core graphite: perspective
journal, December 2013


Three dimensional reconstruction by electron microscopy in the life sciences: An introduction for cell and tissue biologists: T
journal, February 2015

  • Miranda, Kildare; Girard-Dias, Wendell; Attias, Marcia
  • Molecular Reproduction and Development, Vol. 82, Issue 7-8
  • DOI: 10.1002/mrd.22455

Advances in 3D focused ion beam tomography
journal, April 2014


Assessing the utility of FIB-SEM images for shale digital rock physics
journal, September 2016


On the importance of FIB-SEM specific segmentation algorithms for porous media
journal, September 2014


Characterisation of the porous structure of Gilsocarbon graphite using pycnometry, cyclic porosimetry and void-network modeling
journal, July 2014


Thermophysical property and pore structure evolution in stressed and non-stressed neutron irradiated IG-110 nuclear graphite
journal, August 2016


Multi-scale characterization of porosity in Boom Clay (HADES-level, Mol, Belgium) using a combination of X-ray μ-CT, 2D BIB-SEM and FIB-SEM tomography
journal, May 2015


3D Cellular Automata fracture model for porous graphite microstructures
journal, November 2017


Development of evaluation method with X-ray tomography for material property of IG-430 graphite for VHTR/HTGR
journal, May 2014


Large-scale numerical simulation of mechanical and thermal properties of nuclear graphite using a microstructure-based model
journal, December 2008


Microstructural modelling of nuclear graphite using multi-phase models
journal, October 2008


Numerical modelling of the effects of porosity changes on the mechanical properties of nuclear graphite
journal, June 2006


3D characterization and quantitative evaluation of pore-fracture networks of two Chinese coals using FIB-SEM tomography
journal, April 2017


Works referencing / citing this record:

A Review of Finite Element Method Models for Nuclear Graphite Applications
journal, December 2018

  • Arregui-Mena, José David; Worth, Robert N.; Hall, Graham
  • Archives of Computational Methods in Engineering, Vol. 27, Issue 1
  • DOI: 10.1007/s11831-018-09310-y