Correlative X-ray micro-nanotomography with scanning electron microscopy at the Advanced Light Source

Bhattacharjee, Arun J.; Lisabeth, Harrison P.; Parkinson, Dilworth; MacDowell, Alastair

doi:10.1107/S1600577524009305

Correlative X-ray micro-nanotomography with scanning electron microscopy at the Advanced Light Source

Journal Article · Tue Oct 29 00:00:00 EDT 2024 · Journal of Synchrotron Radiation (Online)

DOI:https://doi.org/10.1107/S1600577524009305· OSTI ID:2475201

; Lisabeth, Harrison P.; ; MacDowell, Alastair

Geological samples are inherently multi-scale. Understanding their bulk physical and chemical properties requires characterization down to the nano-scale. A powerful technique to study the three-dimensional microstructure is X-ray tomography, but it lacks information about the chemistry of samples. To develop a methodology for measuring the multi-scale 3D microstructure of geological samples, correlative X-ray micro- and nanotomography were performed on two rocks followed by scanning electron microscopy with energy-dispersive spectroscopy (SEM-EDS) analysis. The study was performed in five steps: (i) micro X-ray tomography was performed on rock sample cores, (ii) samples for nanotomography were prepared using laser milling, (iii) nanotomography was performed on the milled sub-samples, (iv) samples were mounted and polished for SEM analysis and (v) SEM imaging and compositional mapping was performed on micro and nanotomography samples for complimentary information. Correlative study performed on samples of serpentine and basalt revealed multiscale 3D structures involving both solid mineral phases and pore networks. Significant differences in the volume fraction of pores and mineral phases were also observed dependent on the imaging spatial resolution employed. This highlights the necessity for the application of such a multiscale approach for the characterization of complex aggregates such as rocks. Information acquired from the chemical mapping of different phases was also helpful in segmentation of phases that did not exhibit significant contrast in X-ray imaging. Adoption of the protocol used in this study can be broadly applied to 3D imaging studies being performed at the Advanced Light Source and other user facilities.

View Journal Article

Sponsoring Organization:: USDOE

Grant/Contract Number:: AC02-05CH11231

OSTI ID:: 2475201

Alternate ID(s):: OSTI ID: 2497750

Journal Information:: Journal of Synchrotron Radiation (Online), Journal Name: Journal of Synchrotron Radiation (Online) Journal Issue: 6 Vol. 31; ISSN 1600-5775; ISSN JSYRES

Publisher:: International Union of Crystallography (IUCr)Copyright Statement

Country of Publication:: Denmark

Language:: English

References (38)

Multiscale pore structure and its effect on gas transport in organic-rich shale: PORE STRUCTURE AND TRANSPORT IN SHALE Wu, Tianhao; Li, Xiang; Zhao, Junliang Water Resources Research, Vol. 53, Issue 7 https://doi.org/10.1002/2017WR020780	journal	July 2017
3D Visualization of Morphological Evolution of Large Defects during Spark Plasma Sintering of Alumina Granules Okuma, Gaku; Endo, Masaya; Minagawa, Haruki Advanced Engineering Materials, Vol. 25, Issue 18 https://doi.org/10.1002/adem.202201534	journal	March 2023
In Situ Experiments with X ray Tomography: an Attractive Tool for Experimental Mechanics Buffiere, J. -Y.; Maire, E.; Adrien, J. Experimental Mechanics, Vol. 50, Issue 3 https://doi.org/10.1007/s11340-010-9333-7	journal	January 2010
A chemical model for generating the sources of mare basalts: Combined equilibrium and fractional crystallization of the lunar magmasphere Snyder, Gregory A.; Taylor, Lawrence A.; Neal, Clive R. Geochimica et Cosmochimica Acta, Vol. 56, Issue 10 https://doi.org/10.1016/0016-7037(92)90172-F	journal	October 1992
Rare earth element concentrations in geological and synthetic samples using synchrotron X-ray fluorescence analysis Chen, J. R.; Chao, E. C. T.; Back, J. M. Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms, Vol. 75, Issue 1-4 https://doi.org/10.1016/0168-583X(93)95718-K	journal	April 1993
4D synchrotron X-ray tomographic quantification of the transition from cellular to dendrite growth during directional solidification Cai, B.; Wang, J.; Kao, A. Acta Materialia, Vol. 117 https://doi.org/10.1016/j.actamat.2016.07.002	journal	September 2016
In situ synchrotron X-ray micro-tomography study of pitting corrosion in stainless steel Ghahari, S. Majid; Davenport, Alison J.; Rayment, Trevor Corrosion Science, Vol. 53, Issue 9 https://doi.org/10.1016/j.corsci.2011.05.040	journal	September 2011
High-resolution X-ray computed tomography in geosciences: A review of the current technology and applications Cnudde, V.; Boone, M. N. Earth-Science Reviews, Vol. 123 https://doi.org/10.1016/j.earscirev.2013.04.003	journal	August 2013
Current developments and applications of micro-CT for the 3D analysis of multiphase mineral systems in geometallurgy Wang, Y.; Miller, J. D. Earth-Science Reviews, Vol. 211 https://doi.org/10.1016/j.earscirev.2020.103406	journal	December 2020
A review of the application of X-ray computed tomography to the study of coal Mathews, Jonathan P.; Campbell, Quentin P.; Xu, Hao Fuel, Vol. 209 https://doi.org/10.1016/j.fuel.2017.07.079	journal	December 2017
Mineral sequestration of carbon dioxide in basalt: A pre-injection overview of the CarbFix project Gislason, Sigurdur Reynir; Wolff-Boenisch, Domenik; Stefansson, Andri International Journal of Greenhouse Gas Control, Vol. 4, Issue 3 https://doi.org/10.1016/j.ijggc.2009.11.013	journal	May 2010
Correlative core- to pore-scale imaging of shales Goral, Jan; Andrew, Matthew; Olson, Terrilyn Marine and Petroleum Geology, Vol. 111 https://doi.org/10.1016/j.marpetgeo.2019.08.009	journal	January 2020
Microstructural characterization and mechanical behavior of Aba Panu meteorite by correlative microscopy and nanoindentation Huang, Tai-Jan; Niverty, Sridhar; Sundar, Arun Materials Characterization, Vol. 205 https://doi.org/10.1016/j.matchar.2023.113331	journal	November 2023
A guide to synchrotron hard X-ray fluorescence mapping of annually laminated stalagmites: Sample preparation, analysis and evaluation Borsato, Andrea; Frisia, Silvia; Howard, Daryl Spectrochimica Acta Part B: Atomic Spectroscopy, Vol. 185 https://doi.org/10.1016/j.sab.2021.106308	journal	November 2021
Atomic Perspective on the Serpentine–Chlorite Solid-State Transformation Zhang, Hui; Gilbert, Benjamin; Banfield, Jillian F. Chemistry of Materials, Vol. 33, Issue 16 https://doi.org/10.1021/acs.chemmater.1c00894	journal	August 2021
Ultrahigh-Resolution 3D Imaging for Quantifying the Pore Nanostructure of Shale and Predicting Gas Transport Garum, Mohamed; Glover, Paul W. J.; Lorinczi, Piroska Energy & Fuels, Vol. 35, Issue 1 https://doi.org/10.1021/acs.energyfuels.0c03225	journal	December 2020
Dynamic control on serpentine crystallization in veins: Constraints on hydration processes in oceanic peridotites: SERPENTINE CRYSTALLIZATION Andreani, M.; Mével, C.; Boullier, A. -M. Geochemistry, Geophysics, Geosystems, Vol. 8, Issue 2 https://doi.org/10.1029/2006GC001373	journal	February 2007
Petrology of the Apollo 11 ilmenite basalts James, Odette B.; Jackson, Everett D. Journal of Geophysical Research, Vol. 75, Issue 29 https://doi.org/10.1029/JB075i029p05793	journal	October 1970
Correlative single-cell hard X-ray computed tomography and X-ray fluorescence imaging Lin, Zihan; Zhang, Xiao; Nandi, Purbasha Communications Biology, Vol. 7, Issue 1 https://doi.org/10.1038/s42003-024-05950-y	journal	March 2024
High-energy x-ray nanotomography introducing an apodization Fresnel zone plate objective lens Takeuchi, Akihisa; Uesugi, Kentaro; Uesugi, Masayuki Review of Scientific Instruments, Vol. 92, Issue 2 https://doi.org/10.1063/5.0020293	journal	February 2021
X-ray zooming microscopy with two Fresnel zone plates Wakabayashi, Daisuke; Suzuki, Yoshio; Shibazaki, Yuki Review of Scientific Instruments, Vol. 93, Issue 3 https://doi.org/10.1063/5.0070720	journal	March 2022
The hard x-ray nanotomography microscope at the advanced light source Nichols, Joseph B.; Voltolini, Marco; Gilbert, Benjamin Review of Scientific Instruments, Vol. 93, Issue 2 https://doi.org/10.1063/5.0076322	journal	February 2022
A 1300 K furnace forin situX-ray microtomography Bellet, D.; Gorges, B.; Dallery, A. Journal of Applied Crystallography, Vol. 36, Issue 2 https://doi.org/10.1107/S0021889803001158	journal	March 2003
TomoPy: a framework for the analysis of synchrotron tomographic data Gürsoy, Dogˇa; De Carlo, Francesco; Xiao, Xianghui Journal of Synchrotron Radiation, Vol. 21, Issue 5 https://doi.org/10.1107/S1600577514013939	journal	August 2014
A novel high-temperature furnace for combinedin situsynchrotron X-ray diffraction and infrared thermal imaging to investigate the effects of thermal gradients upon the structure of ceramic materials Robinson, James B.; Brown, Leon D.; Jervis, Rhodri Journal of Synchrotron Radiation, Vol. 21, Issue 5 https://doi.org/10.1107/S1600577514014209	journal	August 2014
Real-time streaming tomographic reconstruction with on-demand data capturing and 3D zooming to regions of interest Nikitin, Viktor; Tekawade, Aniket; Duchkov, Anton Journal of Synchrotron Radiation, Vol. 29, Issue 3 https://doi.org/10.1107/S1600577522003095	journal	April 2022
Synchrotron X‐ray multiscale tomography: Visualization of heterogeneous microstructures and defects in ceramics Okuma, Gaku; Wakai, Fumihiro Journal of the American Ceramic Society, Vol. 107, Issue 3 https://doi.org/10.1111/jace.19366	journal	August 2023
Laser-preparation of geometrically optimised samples for X-ray nano-CT: LASER-PREPARATION OF GEOMETRICALLY OPTIMISED SAMPLES FOR X-RAY NANO-CT Bailey, J. J.; Heenan, T. M. M.; Finegan, D. P. Journal of Microscopy, Vol. 267, Issue 3 https://doi.org/10.1111/jmi.12577	journal	May 2017
Developments in synchrotron x-ray computed microtomography at the National Synchrotron Light Source Dowd, Betsy A.; Campbell, Graham H.; Marr, Robert B. SPIE's International Symposium on Optical Science, Engineering, and Instrumentation, SPIE Proceedings https://doi.org/10.1117/12.363725	conference	September 1999
X-ray micro-tomography at the Advanced Light Source MacDowell, A. A.; Parkinson, D. Y.; Haboub, A. SPIE Optical Engineering + Applications, SPIE Proceedings https://doi.org/10.1117/12.930243	conference	October 2012
Silicate Liquid Immiscibility in Lunar Magmas, Evidenced by Melt Inclusions in Lunar Rocks Roedder, Edwin; Weiblen, Paul W. Science, Vol. 167, Issue 3918 https://doi.org/10.1126/science.167.3918.641	journal	January 1970
Improved imaging and analysis of chlorite in reservoirs and modern day analogues: new insights for reservoir quality and provenance Worden, R. H.; Utley, James E. P.; Butcher, Alan R. Geological Society, London, Special Publications, Vol. 484, Issue 1 https://doi.org/10.1144/SP484.10	journal	January 2018
Correlative X-ray Tomographic Imaging of Catalyst Layer Degradation in Fuel Cells White, Robin T.; Ramani, Dilip; Eberhardt, Sebastian Journal of The Electrochemical Society, Vol. 166, Issue 13 https://doi.org/10.1149/2.0121913jes	journal	January 2019
Recent advances in X-ray microtomography applied to materials Stock, S. R. International Materials Reviews, Vol. 53, Issue 3 https://doi.org/10.1179/174328008X277803	journal	May 2008
Secondary Mineral Genesis from Chlorite and Serpentine in an Ultramafic Soil Toposequence Lee, B. D.; Sears, S. K.; Graham, R. C. Soil Science Society of America Journal, Vol. 67, Issue 4 https://doi.org/10.2136/sssaj2003.1309	journal	July 2003
Formation of regularly interstratified serpentine-chlorite minerals by tetrahedral inversion in long-period serpentine polytypes Banfield, Jillian F.; Bailey, Sturges W. American Mineralogist, Vol. 81, Issue 1-2 https://doi.org/10.2138/am-1996-1-211	journal	February 1996
In-Line Phase-Contrast X-ray Imaging and Tomography for Materials Science Mayo, Sheridan C.; Stevenson, Andrew W.; Wilkins, Stephen W. Materials, Vol. 5, Issue 12 https://doi.org/10.3390/ma5050937	journal	May 2012
Application of X-ray computed tomography to soil science: A literature review Taina, I. A.; Heck, R. J.; Elliot, T. R. Canadian Journal of Soil Science, Vol. 88, Issue 1 https://doi.org/10.4141/CJSS06027	journal	February 2008

Similar Records

Comparison of SOFC Cathode Microstructure Quantified using X-ray Nanotomography and Focused Ioni Beam-scanning Electron Microscopy

Journal Article · Fri Dec 30 23:00:00 EST 2011 · Electrochemistry Communications · OSTI ID:1041833

Measurement of accessible reactive surface area in a sandstone, with application to CO2 mineralization

Journal Article · · Chemical Geology · OSTI ID:1066936

Correlative X-ray micro-nanotomography with scanning electron microscopy at the Advanced Light Source

Citation Formats

References (38)

Similar Records

Related Subjects