Correlative X-ray micro-nanotomography with scanning electron microscopy at the Advanced Light Source
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....
Saved in:
| Main Authors: | , , , |
|---|---|
| Format: | Article |
| Language: | English |
| Published: |
International Union of Crystallography
2024-11-01
|
| Series: | Journal of Synchrotron Radiation |
| Subjects: | |
| Online Access: | https://journals.iucr.org/paper?S1600577524009305 |
| Tags: |
Add Tag
No Tags, Be the first to tag this record!
|
| _version_ | 1850198937700401152 |
|---|---|
| author | Arun J. Bhattacharjee Harrison P. Lisabeth Dilworth Parkinson Alastair MacDowell |
| author_facet | Arun J. Bhattacharjee Harrison P. Lisabeth Dilworth Parkinson Alastair MacDowell |
| author_sort | Arun J. Bhattacharjee |
| collection | DOAJ |
| description | 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. |
| format | Article |
| id | doaj-art-cec492b216034a09b5e0ec2a8a07ed01 |
| institution | OA Journals |
| issn | 1600-5775 |
| language | English |
| publishDate | 2024-11-01 |
| publisher | International Union of Crystallography |
| record_format | Article |
| series | Journal of Synchrotron Radiation |
| spelling | doaj-art-cec492b216034a09b5e0ec2a8a07ed012025-08-20T02:12:45ZengInternational Union of CrystallographyJournal of Synchrotron Radiation1600-57752024-11-013161561157010.1107/S1600577524009305vl5028Correlative X-ray micro-nanotomography with scanning electron microscopy at the Advanced Light SourceArun J. Bhattacharjee0Harrison P. Lisabeth1Dilworth Parkinson2Alastair MacDowell3Energy Geosciences Division, Lawrence Berkeley National Laboratory, 1 Cyclotron Rd, Berkeley, CA 94720, USAEnergy Geosciences Division, Lawrence Berkeley National Laboratory, 1 Cyclotron Rd, Berkeley, CA 94720, USAAdvanced Light Source, Lawrence Berkeley National Laboratory, 1 Cyclotron Rd, Berkeley, CA 94720, USAAdvanced Light Source, Lawrence Berkeley National Laboratory, 1 Cyclotron Rd, Berkeley, CA 94720, USAGeological 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.https://journals.iucr.org/paper?S1600577524009305x-ray tomographyscanning electron microscopybasaltserpentiniteenergy-dispersive x-ray spectroscopy |
| spellingShingle | Arun J. Bhattacharjee Harrison P. Lisabeth Dilworth Parkinson Alastair MacDowell Correlative X-ray micro-nanotomography with scanning electron microscopy at the Advanced Light Source Journal of Synchrotron Radiation x-ray tomography scanning electron microscopy basalt serpentinite energy-dispersive x-ray spectroscopy |
| title | Correlative X-ray micro-nanotomography with scanning electron microscopy at the Advanced Light Source |
| title_full | Correlative X-ray micro-nanotomography with scanning electron microscopy at the Advanced Light Source |
| title_fullStr | Correlative X-ray micro-nanotomography with scanning electron microscopy at the Advanced Light Source |
| title_full_unstemmed | Correlative X-ray micro-nanotomography with scanning electron microscopy at the Advanced Light Source |
| title_short | Correlative X-ray micro-nanotomography with scanning electron microscopy at the Advanced Light Source |
| title_sort | correlative x ray micro nanotomography with scanning electron microscopy at the advanced light source |
| topic | x-ray tomography scanning electron microscopy basalt serpentinite energy-dispersive x-ray spectroscopy |
| url | https://journals.iucr.org/paper?S1600577524009305 |
| work_keys_str_mv | AT arunjbhattacharjee correlativexraymicronanotomographywithscanningelectronmicroscopyattheadvancedlightsource AT harrisonplisabeth correlativexraymicronanotomographywithscanningelectronmicroscopyattheadvancedlightsource AT dilworthparkinson correlativexraymicronanotomographywithscanningelectronmicroscopyattheadvancedlightsource AT alastairmacdowell correlativexraymicronanotomographywithscanningelectronmicroscopyattheadvancedlightsource |