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Methods to expose subsurface objects of interest identified from 3D imaging: The intermediate sample preparation stage in the correlative microscopy workflow

Ria Mitchell Orcid Logo, Tom Dunlop Orcid Logo, T. Volkenandt, J. Russell, P. Davies, S. Spooner, Cameron Pleydell-Pearce, Richard Johnston Orcid Logo

Journal of Microscopy, Volume: 289, Issue: 2, Pages: 107 - 127

Swansea University Authors: Ria Mitchell Orcid Logo, Tom Dunlop Orcid Logo, Cameron Pleydell-Pearce, Richard Johnston Orcid Logo

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DOI (Published version): 10.1111/jmi.13159

Abstract

The correlative imaging workflow is a method of combining information and data across modes (e.g. SEM, X-ray CT, FIB-SEM), scales (cm to nm) and dimensions (2D–3D–4D), providing a more holistic interpretation of the research question. Often, subsurface objects of interest (e.g. inclusions, pores, cr...

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Published in: Journal of Microscopy
ISSN: 0022-2720 1365-2818
Published: Wiley 2023
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URI: https://cronfa.swan.ac.uk/Record/cronfa64709
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Often, subsurface objects of interest (e.g. inclusions, pores, cracks, defects in multilayered samples) are identified from initial exploratory nondestructive 3D tomographic imaging (e.g. X-ray CT, XRM), and those objects need to be studied using additional techniques to obtain, for example, 2D chemical or crystallographic data. Consequently, an intermediate sample preparation step needs to be completed, where a targeted amount of sample surface material is removed, exposing and revealing the object of interest. At present, there is not one singular technique for removing varied thicknesses at high resolution and on a range of scales from cm to nm. Here, we review the manual and automated options currently available for targeted sample material removal, with a focus on those methods which are readily accessible in most laboratories. We summarise the approaches for manual grinding and polishing, automated grinding and polishing, microtome/ultramicrotome, and broad-beam ion milling (BBIM), with further review of other more specialist techniques including serial block face electron microscopy (SBF-SEM), and ion milling and laser approaches such as FIB-SEM, Xe plasma FIB-SEM, and femtosecond laser/LaserFIB. We also address factors which may influence the decision on a particular technique, including the composition, shape and size of the samples, sample mounting limitations, the amount of surface material to be removed, the accuracy and/or resolution of peripheral parts, the accuracy and/or resolution of the technique/instrumentation, and other more general factors such as accessibility to instrumentation, costs, and the time taken for experimentation. It is hoped that this study will provide researchers with a range of options for removal of specific amounts of sample surface material to reach subsurface objects of interest in both correlative and non-correlative workflows.</abstract><type>Journal Article</type><journal>Journal of Microscopy</journal><volume>289</volume><journalNumber>2</journalNumber><paginationStart>107</paginationStart><paginationEnd>127</paginationEnd><publisher>Wiley</publisher><placeOfPublication/><isbnPrint/><isbnElectronic/><issnPrint>0022-2720</issnPrint><issnElectronic>1365-2818</issnElectronic><keywords>Correlative imaging, microscopy, sample preparation, tomography</keywords><publishedDay>1</publishedDay><publishedMonth>2</publishedMonth><publishedYear>2023</publishedYear><publishedDate>2023-02-01</publishedDate><doi>10.1111/jmi.13159</doi><url>http://dx.doi.org/10.1111/jmi.13159</url><notes/><college>COLLEGE NANME</college><department>Engineering</department><CollegeCode>COLLEGE CODE</CollegeCode><DepartmentCode>EEN</DepartmentCode><institution>Swansea University</institution><apcterm/><funders>EPSRC</funders><projectreference>EP/M028267/1, EP/T006390/1</projectreference><lastEdited>2023-12-01T14:58:37.0314002</lastEdited><Created>2023-10-11T11:32:10.1145190</Created><path><level id="1">Faculty of Science and Engineering</level><level id="2">School of Engineering and Applied Sciences - Materials Science and Engineering</level></path><authors><author><firstname>Ria</firstname><surname>Mitchell</surname><orcid>0000-0002-6328-3998</orcid><order>1</order></author><author><firstname>Tom</firstname><surname>Dunlop</surname><orcid>0000-0002-5851-8713</orcid><order>2</order></author><author><firstname>T.</firstname><surname>Volkenandt</surname><order>3</order></author><author><firstname>J.</firstname><surname>Russell</surname><order>4</order></author><author><firstname>P.</firstname><surname>Davies</surname><order>5</order></author><author><firstname>S.</firstname><surname>Spooner</surname><order>6</order></author><author><firstname>Cameron</firstname><surname>Pleydell-Pearce</surname><orcid/><order>7</order></author><author><firstname>Richard</firstname><surname>Johnston</surname><orcid>0000-0003-1977-6418</orcid><order>8</order></author></authors><documents/><OutputDurs/></rfc1807>
spelling v2 64709 2023-10-11 Methods to expose subsurface objects of interest identified from 3D imaging: The intermediate sample preparation stage in the correlative microscopy workflow fcfffafbafb0036c483338f839df45e5 0000-0002-6328-3998 Ria Mitchell Ria Mitchell true false 809395460ab1e6b53a906b136d919c41 0000-0002-5851-8713 Tom Dunlop Tom Dunlop true false 564c480cb2abe761533a139c7dbaaca1 Cameron Pleydell-Pearce Cameron Pleydell-Pearce true false 23282e7acce87dd926b8a62ae410a393 0000-0003-1977-6418 Richard Johnston Richard Johnston true false 2023-10-11 EEN The correlative imaging workflow is a method of combining information and data across modes (e.g. SEM, X-ray CT, FIB-SEM), scales (cm to nm) and dimensions (2D–3D–4D), providing a more holistic interpretation of the research question. Often, subsurface objects of interest (e.g. inclusions, pores, cracks, defects in multilayered samples) are identified from initial exploratory nondestructive 3D tomographic imaging (e.g. X-ray CT, XRM), and those objects need to be studied using additional techniques to obtain, for example, 2D chemical or crystallographic data. Consequently, an intermediate sample preparation step needs to be completed, where a targeted amount of sample surface material is removed, exposing and revealing the object of interest. At present, there is not one singular technique for removing varied thicknesses at high resolution and on a range of scales from cm to nm. Here, we review the manual and automated options currently available for targeted sample material removal, with a focus on those methods which are readily accessible in most laboratories. We summarise the approaches for manual grinding and polishing, automated grinding and polishing, microtome/ultramicrotome, and broad-beam ion milling (BBIM), with further review of other more specialist techniques including serial block face electron microscopy (SBF-SEM), and ion milling and laser approaches such as FIB-SEM, Xe plasma FIB-SEM, and femtosecond laser/LaserFIB. We also address factors which may influence the decision on a particular technique, including the composition, shape and size of the samples, sample mounting limitations, the amount of surface material to be removed, the accuracy and/or resolution of peripheral parts, the accuracy and/or resolution of the technique/instrumentation, and other more general factors such as accessibility to instrumentation, costs, and the time taken for experimentation. It is hoped that this study will provide researchers with a range of options for removal of specific amounts of sample surface material to reach subsurface objects of interest in both correlative and non-correlative workflows. Journal Article Journal of Microscopy 289 2 107 127 Wiley 0022-2720 1365-2818 Correlative imaging, microscopy, sample preparation, tomography 1 2 2023 2023-02-01 10.1111/jmi.13159 http://dx.doi.org/10.1111/jmi.13159 COLLEGE NANME Engineering COLLEGE CODE EEN Swansea University EPSRC EP/M028267/1, EP/T006390/1 2023-12-01T14:58:37.0314002 2023-10-11T11:32:10.1145190 Faculty of Science and Engineering School of Engineering and Applied Sciences - Materials Science and Engineering Ria Mitchell 0000-0002-6328-3998 1 Tom Dunlop 0000-0002-5851-8713 2 T. Volkenandt 3 J. Russell 4 P. Davies 5 S. Spooner 6 Cameron Pleydell-Pearce 7 Richard Johnston 0000-0003-1977-6418 8
title Methods to expose subsurface objects of interest identified from 3D imaging: The intermediate sample preparation stage in the correlative microscopy workflow
spellingShingle Methods to expose subsurface objects of interest identified from 3D imaging: The intermediate sample preparation stage in the correlative microscopy workflow
Ria Mitchell
Tom Dunlop
Cameron Pleydell-Pearce
Richard Johnston
title_short Methods to expose subsurface objects of interest identified from 3D imaging: The intermediate sample preparation stage in the correlative microscopy workflow
title_full Methods to expose subsurface objects of interest identified from 3D imaging: The intermediate sample preparation stage in the correlative microscopy workflow
title_fullStr Methods to expose subsurface objects of interest identified from 3D imaging: The intermediate sample preparation stage in the correlative microscopy workflow
title_full_unstemmed Methods to expose subsurface objects of interest identified from 3D imaging: The intermediate sample preparation stage in the correlative microscopy workflow
title_sort Methods to expose subsurface objects of interest identified from 3D imaging: The intermediate sample preparation stage in the correlative microscopy workflow
author_id_str_mv fcfffafbafb0036c483338f839df45e5
809395460ab1e6b53a906b136d919c41
564c480cb2abe761533a139c7dbaaca1
23282e7acce87dd926b8a62ae410a393
author_id_fullname_str_mv fcfffafbafb0036c483338f839df45e5_***_Ria Mitchell
809395460ab1e6b53a906b136d919c41_***_Tom Dunlop
564c480cb2abe761533a139c7dbaaca1_***_Cameron Pleydell-Pearce
23282e7acce87dd926b8a62ae410a393_***_Richard Johnston
author Ria Mitchell
Tom Dunlop
Cameron Pleydell-Pearce
Richard Johnston
author2 Ria Mitchell
Tom Dunlop
T. Volkenandt
J. Russell
P. Davies
S. Spooner
Cameron Pleydell-Pearce
Richard Johnston
format Journal article
container_title Journal of Microscopy
container_volume 289
container_issue 2
container_start_page 107
publishDate 2023
institution Swansea University
issn 0022-2720
1365-2818
doi_str_mv 10.1111/jmi.13159
publisher Wiley
college_str Faculty of Science and Engineering
hierarchytype
hierarchy_top_id facultyofscienceandengineering
hierarchy_top_title Faculty of Science and Engineering
hierarchy_parent_id facultyofscienceandengineering
hierarchy_parent_title Faculty of Science and Engineering
department_str School of Engineering and Applied Sciences - Materials Science and Engineering{{{_:::_}}}Faculty of Science and Engineering{{{_:::_}}}School of Engineering and Applied Sciences - Materials Science and Engineering
url http://dx.doi.org/10.1111/jmi.13159
document_store_str 0
active_str 0
description The correlative imaging workflow is a method of combining information and data across modes (e.g. SEM, X-ray CT, FIB-SEM), scales (cm to nm) and dimensions (2D–3D–4D), providing a more holistic interpretation of the research question. Often, subsurface objects of interest (e.g. inclusions, pores, cracks, defects in multilayered samples) are identified from initial exploratory nondestructive 3D tomographic imaging (e.g. X-ray CT, XRM), and those objects need to be studied using additional techniques to obtain, for example, 2D chemical or crystallographic data. Consequently, an intermediate sample preparation step needs to be completed, where a targeted amount of sample surface material is removed, exposing and revealing the object of interest. At present, there is not one singular technique for removing varied thicknesses at high resolution and on a range of scales from cm to nm. Here, we review the manual and automated options currently available for targeted sample material removal, with a focus on those methods which are readily accessible in most laboratories. We summarise the approaches for manual grinding and polishing, automated grinding and polishing, microtome/ultramicrotome, and broad-beam ion milling (BBIM), with further review of other more specialist techniques including serial block face electron microscopy (SBF-SEM), and ion milling and laser approaches such as FIB-SEM, Xe plasma FIB-SEM, and femtosecond laser/LaserFIB. We also address factors which may influence the decision on a particular technique, including the composition, shape and size of the samples, sample mounting limitations, the amount of surface material to be removed, the accuracy and/or resolution of peripheral parts, the accuracy and/or resolution of the technique/instrumentation, and other more general factors such as accessibility to instrumentation, costs, and the time taken for experimentation. It is hoped that this study will provide researchers with a range of options for removal of specific amounts of sample surface material to reach subsurface objects of interest in both correlative and non-correlative workflows.
published_date 2023-02-01T14:58:38Z
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score 11.013148

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