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

Journal Article · 01 December 2018 · Journal of Nuclear Materials

DOI: https://doi.org/10.1016/j.jnucmat.2018.08.047 · OSTI ID:1471932

^[1];

^[1]

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

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.

View Accepted Manuscript (DOE)

Cite

Export

Save

Research Organization:: Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)

Sponsoring Organization:: USDOE

Grant/Contract Number:: AC05-00OR22725

OSTI ID:: 1471932

Journal Information:: Journal of Nuclear Materials, Journal Name: Journal of Nuclear Materials Journal Issue: C Vol. 511; ISSN 0022-3115

Publisher:: ElsevierCopyright Statement

Country of Publication:: United States

Language:: English

References (25)

Three dimensional reconstruction by electron microscopy in the life sciences: An introduction for cell and tissue biologists: T Miranda, Kildare; Girard-Dias, Wendell; Attias, Marcia Molecular Reproduction and Development, Vol. 82, Issue 7-8 https://doi.org/10.1002/mrd.22455	journal	February 2015
Microstructure of carbon blacks in pitch-bonded graphites and structural changes produced by gas—graphite oxidation reactions Jones, S. S.; Woodruff, E. M. Carbon, Vol. 9, Issue 3 https://doi.org/10.1016/0008-6223(71)90044-3	journal	May 1971
Assessing the utility of FIB-SEM images for shale digital rock physics Kelly, Shaina; El-Sobky, Hesham; Torres-Verdín, Carlos Advances in Water Resources, Vol. 95 https://doi.org/10.1016/j.advwatres.2015.06.010	journal	September 2016
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 Saif, Tarik; Lin, Qingyang; Butcher, Alan R. Applied Energy, Vol. 202 https://doi.org/10.1016/j.apenergy.2017.05.039	journal	September 2017
The microstructure of nuclear graphite binders Wen, K. Y.; Marrow, T. J.; Marsden, B. J. Carbon, Vol. 46, Issue 1 https://doi.org/10.1016/j.carbon.2007.10.025	journal	January 2008
Characterisation of the porous structure of Gilsocarbon graphite using pycnometry, cyclic porosimetry and void-network modeling Laudone, Giuliano M.; Gribble, Christopher M.; Matthews, G. Peter Carbon, Vol. 73 https://doi.org/10.1016/j.carbon.2014.02.037	journal	July 2014
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 Houben, M. E.; Desbois, G.; Urai, J. L. Applied Clay Science, Vol. 71 https://doi.org/10.1016/j.clay.2012.11.006	journal	January 2013
3D characterization and quantitative evaluation of pore-fracture networks of two Chinese coals using FIB-SEM tomography Zhou, Sandong; Liu, Dameng; Cai, Yidong International Journal of Coal Geology, Vol. 174 https://doi.org/10.1016/j.coal.2017.03.008	journal	April 2017
Numerical modelling of the effects of porosity changes on the mechanical properties of nuclear graphite Berre, C.; Fok, S. L.; Marsden, B. J. Journal of Nuclear Materials, Vol. 352, Issue 1-3 https://doi.org/10.1016/j.jnucmat.2006.02.037	journal	June 2006
Microstructural modelling of nuclear graphite using multi-phase models Berre, C.; Fok, S. L.; Marsden, B. J. Journal of Nuclear Materials, Vol. 380, Issue 1-3 https://doi.org/10.1016/j.jnucmat.2008.07.006	journal	October 2008
Microstructural characterization and pore structure analysis of nuclear graphite Kane, J.; Karthik, C.; Butt, D. P. Journal of Nuclear Materials, Vol. 415, Issue 2 https://doi.org/10.1016/j.jnucmat.2011.05.053	journal	August 2011
Thermophysical property and pore structure evolution in stressed and non-stressed neutron irradiated IG-110 nuclear graphite Snead, L. L.; Contescu, C. I.; Byun, T. S. Journal of Nuclear Materials, Vol. 476 https://doi.org/10.1016/j.jnucmat.2016.04.042	journal	August 2016
On the importance of FIB-SEM specific segmentation algorithms for porous media Salzer, Martin; Thiele, Simon; Zengerle, Roland Materials Characterization, Vol. 95 https://doi.org/10.1016/j.matchar.2014.05.014	journal	September 2014
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 Hemes, Susanne; Desbois, Guillaume; Urai, Janos L. Microporous and Mesoporous Materials, Vol. 208 https://doi.org/10.1016/j.micromeso.2015.01.022	journal	May 2015
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) Bera, Bijoyendra; Mitra, Sushanta K.; Vick, Douglas Micron, Vol. 42, Issue 5 https://doi.org/10.1016/j.micron.2010.12.002	journal	July 2011
Large-scale numerical simulation of mechanical and thermal properties of nuclear graphite using a microstructure-based model Wang, H. T.; Yu, S. Y. Nuclear Engineering and Design, Vol. 238, Issue 12 https://doi.org/10.1016/j.nucengdes.2008.07.003	journal	December 2008
Overview of strength, crack propagation and fracture of nuclear reactor moderator graphite Moskovic, R.; Heard, P. J.; Flewitt, P. E. J. Nuclear Engineering and Design, Vol. 263 https://doi.org/10.1016/j.nucengdes.2013.05.011	journal	October 2013
Development of evaluation method with X-ray tomography for material property of IG-430 graphite for VHTR/HTGR Sumita, Junya; Shibata, Taiju; Fujita, Ichiro Nuclear Engineering and Design, Vol. 271 https://doi.org/10.1016/j.nucengdes.2013.11.053	journal	May 2014
3D Cellular Automata fracture model for porous graphite microstructures Vertyagina, Yelena; Marrow, Thomas James Nuclear Engineering and Design, Vol. 323 https://doi.org/10.1016/j.nucengdes.2016.10.015	journal	November 2017
Secondary ion mass spectrometric image depth profiling for three-dimensional elemental analysis Patkin, Adam J.; Morrison, George H. Analytical Chemistry, Vol. 54, Issue 1 https://doi.org/10.1021/ac00238a005	journal	January 1982
Subsurface nanoindentation deformation of Cu-Al multilayers mapped in 3D by focused ion beam microscopy Inkson, B. J.; Steer, T.; Mobus, G. Journal of Microscopy, Vol. 201, Issue 2 https://doi.org/10.1046/j.1365-2818.2001.00767.x	journal	February 2001
Dimensional change, irradiation creep and thermal/mechanical property changes in nuclear graphite Marsden, B. J.; Haverty, M.; Bodel, W. International Materials Reviews, Vol. 61, Issue 3 https://doi.org/10.1080/09506608.2015.1136460	journal	April 2016
Three-dimensional analysis of porous BaTiO3 ceramics using FIB nanotomography Holzer, L.; Indutnyi, F.; Gasser, Ph. Journal of Microscopy, Vol. 216, Issue 1 https://doi.org/10.1111/j.0022-2720.2004.01397.x	journal	October 2004
Understanding fracture behaviour of PGA reactor core graphite: perspective Moskovic, R.; Flewitt, P. E. J.; Schlangen, E. Materials Science and Technology, Vol. 30, Issue 2 https://doi.org/10.1179/1743284713Y.0000000354	journal	December 2013
Advances in 3D focused ion beam tomography Cantoni, Marco; Holzer, Lorenz MRS Bulletin, Vol. 39, Issue 4 https://doi.org/10.1557/mrs.2014.54	journal	April 2014

Cited By (1)

A Review of Finite Element Method Models for Nuclear Graphite Applications Arregui-Mena, José David; Worth, Robert N.; Hall, Graham Archives of Computational Methods in Engineering, Vol. 27, Issue 1 https://doi.org/10.1007/s11831-018-09310-y	journal	December 2018

Linked Research (2)

Similar Records

Pores in Marcellus Shale: A Neutron Scattering and FIB-SEM Study

Journal Article · 2015 · Energy and Fuels · OSTI ID:1279416

Gu, Xin; Cole, David R.; Rother, Gernot; +2 more

Characterization of PyC/SiC interfaces with FIB-SEM tomography

Journal Article · 2020 · Journal of Nuclear Materials · OSTI ID:1777770

Arregui Mena, Jose David; Seibert, Rachel L.; Gerczak, Tyler J.

Enhanced FIB-SEM systems for large-volume 3D imaging

Journal Article · 2017 · eLife · OSTI ID:1363984

Xu, C. Shan; Hayworth, Kenneth J.; Lu, Zhiyuan; +7 more

Related Subjects

36 MATERIALS SCIENCE

Data for: Site specific, high-resolution characterisation of porosity in graphite using FIB-SEM tomography Arregui-Mena, José https://doi.org/10.17632/cgbmz3hd58 The current record is supplemented by this dataset	dataset	January 2018
Data for: Site specific, high-resolution characterisation of porosity in graphite using FIB-SEM tomography Arregui-Mena, José https://doi.org/10.17632/cgbmz3hd58.1 The current record is supplemented by this dataset	dataset	January 2018