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

Arregui-Mena, Jose' D.; Edmondson, Philip D.; Campbell, Anne A.; Katoh, Yutai

doi:10.1016/j.jnucmat.2018.08.047

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:

^[1];

^[1]

Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

Publication Date:: Sat Dec 01 00:00:00 EST 2018

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.

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                    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

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                    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.

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@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}

}

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Works referenced in this record:

The microstructure of nuclear graphite binders
journal, January 2008

Wen, K. Y.; Marrow, T. J.; Marsden, B. J.
Carbon, Vol. 46, Issue 1
DOI: 10.1016/j.carbon.2007.10.025

Microstructure of carbon blacks in pitch-bonded graphites and structural changes produced by gas—graphite oxidation reactions
journal, May 1971

Jones, S. S.; Woodruff, E. M.
Carbon, Vol. 9, Issue 3
DOI: 10.1016/0008-6223(71)90044-3

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

Kane, J.; Karthik, C.; Butt, D. P.
Journal of Nuclear Materials, Vol. 415, Issue 2
DOI: 10.1016/j.jnucmat.2011.05.053

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

Marsden, B. J.; Haverty, M.; Bodel, W.
International Materials Reviews, Vol. 61, Issue 3
DOI: 10.1080/09506608.2015.1136460

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

Inkson, B. J.; Steer, T.; Mobus, G.
Journal of Microscopy, Vol. 201, Issue 2
DOI: 10.1046/j.1365-2818.2001.00767.x

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

Holzer, L.; Indutnyi, F.; Gasser, Ph.
Journal of Microscopy, Vol. 216, Issue 1
DOI: 10.1111/j.0022-2720.2004.01397.x

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

Moskovic, R.; Heard, P. J.; Flewitt, P. E. J.
Nuclear Engineering and Design, Vol. 263
DOI: 10.1016/j.nucengdes.2013.05.011

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

Moskovic, R.; Flewitt, P. E. J.; Schlangen, E.
Materials Science and Technology, Vol. 30, Issue 2
DOI: 10.1179/1743284713Y.0000000354

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

Cantoni, Marco; Holzer, Lorenz
MRS Bulletin, Vol. 39, Issue 4
DOI: 10.1557/mrs.2014.54

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

Kelly, Shaina; El-Sobky, Hesham; Torres-Verdín, Carlos
Advances in Water Resources, Vol. 95
DOI: 10.1016/j.advwatres.2015.06.010

Pore morphology and distribution in the Shaly facies of Opalinus Clay (Mont Terri, Switzerland): Insights from representative 2D BIB–SEM investigations on mm to nm scale
journal, January 2013

Houben, M. E.; Desbois, G.; Urai, J. L.
Applied Clay Science, Vol. 71
DOI: 10.1016/j.clay.2012.11.006

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

Salzer, Martin; Thiele, Simon; Zengerle, Roland
Materials Characterization, Vol. 95
DOI: 10.1016/j.matchar.2014.05.014

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

Laudone, Giuliano M.; Gribble, Christopher M.; Matthews, G. Peter
Carbon, Vol. 73
DOI: 10.1016/j.carbon.2014.02.037

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

Snead, L. L.; Contescu, C. I.; Byun, T. S.
Journal of Nuclear Materials, Vol. 476
DOI: 10.1016/j.jnucmat.2016.04.042

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

Hemes, Susanne; Desbois, Guillaume; Urai, Janos L.
Microporous and Mesoporous Materials, Vol. 208
DOI: 10.1016/j.micromeso.2015.01.022

Multi-scale multi-dimensional microstructure imaging of oil shale pyrolysis using X-ray micro-tomography, automated ultra-high resolution SEM, MAPS Mineralogy and FIB-SEM
journal, September 2017

Saif, Tarik; Lin, Qingyang; Butcher, Alan R.
Applied Energy, Vol. 202
DOI: 10.1016/j.apenergy.2017.05.039

Understanding the micro structure of Berea Sandstone by the simultaneous use of micro-computed tomography (micro-CT) and focused ion beam-scanning electron microscopy (FIB-SEM)
journal, July 2011

Bera, Bijoyendra; Mitra, Sushanta K.; Vick, Douglas
Micron, Vol. 42, Issue 5
DOI: 10.1016/j.micron.2010.12.002

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

Vertyagina, Yelena; Marrow, Thomas James
Nuclear Engineering and Design, Vol. 323
DOI: 10.1016/j.nucengdes.2016.10.015

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

Sumita, Junya; Shibata, Taiju; Fujita, Ichiro
Nuclear Engineering and Design, Vol. 271
DOI: 10.1016/j.nucengdes.2013.11.053

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

Wang, H. T.; Yu, S. Y.
Nuclear Engineering and Design, Vol. 238, Issue 12
DOI: 10.1016/j.nucengdes.2008.07.003

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

Berre, C.; Fok, S. L.; Marsden, B. J.
Journal of Nuclear Materials, Vol. 380, Issue 1-3
DOI: 10.1016/j.jnucmat.2008.07.006

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

Berre, C.; Fok, S. L.; Marsden, B. J.
Journal of Nuclear Materials, Vol. 352, Issue 1-3
DOI: 10.1016/j.jnucmat.2006.02.037

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

Zhou, Sandong; Liu, Dameng; Cai, Yidong
International Journal of Coal Geology, Vol. 174
DOI: 10.1016/j.coal.2017.03.008

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

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

Abstract

Citation Formats

The microstructure of nuclear graphite binders journal, January 2008

Microstructure of carbon blacks in pitch-bonded graphites and structural changes produced by gas—graphite oxidation reactions journal, May 1971

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

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

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

Pore morphology and distribution in the Shaly facies of Opalinus Clay (Mont Terri, Switzerland): Insights from representative 2D BIB–SEM investigations on mm to nm scale journal, January 2013

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

Multi-scale multi-dimensional microstructure imaging of oil shale pyrolysis using X-ray micro-tomography, automated ultra-high resolution SEM, MAPS Mineralogy and FIB-SEM journal, September 2017

Understanding the micro structure of Berea Sandstone by the simultaneous use of micro-computed tomography (micro-CT) and focused ion beam-scanning electron microscopy (FIB-SEM) journal, July 2011

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

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

The microstructure of nuclear graphite binders
journal, January 2008

Microstructure of carbon blacks in pitch-bonded graphites and structural changes produced by gas—graphite oxidation reactions
journal, May 1971

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

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

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

Pore morphology and distribution in the Shaly facies of Opalinus Clay (Mont Terri, Switzerland): Insights from representative 2D BIB–SEM investigations on mm to nm scale
journal, January 2013

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

Multi-scale multi-dimensional microstructure imaging of oil shale pyrolysis using X-ray micro-tomography, automated ultra-high resolution SEM, MAPS Mineralogy and FIB-SEM
journal, September 2017

Understanding the micro structure of Berea Sandstone by the simultaneous use of micro-computed tomography (micro-CT) and focused ion beam-scanning electron microscopy (FIB-SEM)
journal, July 2011

3D Cellular Automata fracture model for porous graphite microstructures
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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
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Numerical modelling of the effects of porosity changes on the mechanical properties of nuclear graphite
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A Review of Finite Element Method Models for Nuclear Graphite Applications
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