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Linking microstructures and performances of functional coatings and engineering materials through multiscale and correlative microscopy methods / JEBIN JESTINE

Swansea University Author: JEBIN JESTINE

DOI (Published version): 10.23889/SUThesis.71460

Abstract

Correlative characterisation workflows linking optical, electron and X-ray microscopy, enable researchers to chain multiple techniques, overcoming the limitations of any one technique. Applying correlative workflows create rich multimodal datasets covering chemical, mechanical and microstructural in...

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Published: Swansea University 2025
Institution: Swansea University
Degree level: Doctoral
Degree name: EngD
Supervisor: Johnston, R., and Pleydell-Pearce, C.
URI: https://cronfa.swan.ac.uk/Record/cronfa71460
first_indexed 2026-02-17T15:34:25Z
last_indexed 2026-02-18T05:35:32Z
id cronfa71460
recordtype RisThesis
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The application of correlative microscopy is becoming more common due to increased availability and improvements to techniques. Careful thought is required to prepare correlative workflows ensuring decisions do not have negative impacts on downstream processes e.g. destructive techniques should not limit further characterisation, if possible. For example, once a sample undergoes milling to prepare a cross section it is not possible to analyse the removed material.This study focusses on two specific applications/materials with differing origins, structures, chemistry and scale to demonstrate potential differences and similarities for users in very different fields. The two applications/materials are carbon-based perovskite solar cells, and thornback ray (Raja clavata) dermal denticle. The reason for selecting these two different materials is because they both have a thin functional layer which presents challenges for characterisation. The conductive layer of the carbon-based perovskite solar cell is around 20 microns, while the outer layer of the dermal denticle is around 30-50 microns.Carbon-based perovskite solar cells offer a low cost, efficient and stable design for photovoltaics. Within this EngD, these multilayered engineered devices have been characterised in 3D for the first time revealing the carbon flake orientations and porosity within the top mesoporous carbon layer and infiltration defects within the active layer. Three workflows of sample preparation and characterisation were designed and employed for these devices, and an optimised workflow was identified.With the carbon-based perovskite solar cell, the correlative workflow consisted of focused ion billing to prepare a pilar for X-ray microtomography, femtosecond laser machining for nano X-ray microscopy and focused ion beam tomography with energy dispersive X-ray spectroscopy. This work has the potential to become part of a feedback loop for researchers in the photovoltaics community, and other applications such as semiconductor technology who are at the cutting edge of pilot-scale manufacture.Dermal denticles of thornback ray comprise of a dentine protrusion with an enamel cap. They were characterised with a correlative workflow for the first time, analysing the chemical, mechanical and microstructural properties to understand how the enamel layer can perform the required function. The correlative workflow for the dermal denticle consisted of optical microscopy, X-ray microtomography, scanning electron microscopy with energy dispersive X-ray spectroscopy, mechanical testing with nanoindentation, in-situ nanoindentation during X-ray microscopy along with computational modelling. The results show the potential function, of enamel as providing a sacrificial layer to protect the dentin body, it can do so with chemical enrichment, mechanically enhanced properties, and an optimised microstructure for wear resistance.This study demonstrates the application and development of correlative workflows for two different applications showcasing challenges and similarities.</abstract><type>E-Thesis</type><journal/><volume/><journalNumber/><paginationStart/><paginationEnd/><publisher/><placeOfPublication>Swansea University</placeOfPublication><isbnPrint/><isbnElectronic/><issnPrint/><issnElectronic/><keywords>Microscopy, workflows, X-ray CT, Electron microscopy, correlative workflows, carbon perovskite solar cells, biological functional layer</keywords><publishedDay>2</publishedDay><publishedMonth>7</publishedMonth><publishedYear>2025</publishedYear><publishedDate>2025-07-02</publishedDate><doi>10.23889/SUThesis.71460</doi><url/><notes/><college>COLLEGE NANME</college><CollegeCode>COLLEGE CODE</CollegeCode><institution>Swansea University</institution><supervisor>Johnston, R., and Pleydell-Pearce, C.</supervisor><degreelevel>Doctoral</degreelevel><degreename>EngD</degreename><degreesponsorsfunders>WEFO</degreesponsorsfunders><apcterm/><funders>WEFO</funders><projectreference/><lastEdited>2026-02-17T15:41:05.1915996</lastEdited><Created>2026-02-17T15:23:44.1771432</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>JEBIN</firstname><surname>JESTINE</surname><order>1</order></author></authors><documents><document><filename>71460__36252__380422a1927f4a36825d79c6430fe3a7.pdf</filename><originalFilename>2024_Jestine_J.final.71460.pdf</originalFilename><uploaded>2026-02-17T15:33:13.0883108</uploaded><type>Output</type><contentLength>134875307</contentLength><contentType>application/pdf</contentType><version>E-Thesis &#x2013; open access</version><cronfaStatus>true</cronfaStatus><documentNotes>Copyright: the author, Jebin Jestine, 2026</documentNotes><copyrightCorrect>true</copyrightCorrect><language>eng</language></document></documents><OutputDurs/></rfc1807>
spelling 2026-02-17T15:41:05.1915996 v2 71460 2026-02-17 Linking microstructures and performances of functional coatings and engineering materials through multiscale and correlative microscopy methods 760a6299a92c64d6d1650ebd6dcd9e4e JEBIN JESTINE JEBIN JESTINE true false 2026-02-17 Correlative characterisation workflows linking optical, electron and X-ray microscopy, enable researchers to chain multiple techniques, overcoming the limitations of any one technique. Applying correlative workflows create rich multimodal datasets covering chemical, mechanical and microstructural information across 2D and 3D, traversing length scales from macro to nanoscale. The application of correlative microscopy is becoming more common due to increased availability and improvements to techniques. Careful thought is required to prepare correlative workflows ensuring decisions do not have negative impacts on downstream processes e.g. destructive techniques should not limit further characterisation, if possible. For example, once a sample undergoes milling to prepare a cross section it is not possible to analyse the removed material.This study focusses on two specific applications/materials with differing origins, structures, chemistry and scale to demonstrate potential differences and similarities for users in very different fields. The two applications/materials are carbon-based perovskite solar cells, and thornback ray (Raja clavata) dermal denticle. The reason for selecting these two different materials is because they both have a thin functional layer which presents challenges for characterisation. The conductive layer of the carbon-based perovskite solar cell is around 20 microns, while the outer layer of the dermal denticle is around 30-50 microns.Carbon-based perovskite solar cells offer a low cost, efficient and stable design for photovoltaics. Within this EngD, these multilayered engineered devices have been characterised in 3D for the first time revealing the carbon flake orientations and porosity within the top mesoporous carbon layer and infiltration defects within the active layer. Three workflows of sample preparation and characterisation were designed and employed for these devices, and an optimised workflow was identified.With the carbon-based perovskite solar cell, the correlative workflow consisted of focused ion billing to prepare a pilar for X-ray microtomography, femtosecond laser machining for nano X-ray microscopy and focused ion beam tomography with energy dispersive X-ray spectroscopy. This work has the potential to become part of a feedback loop for researchers in the photovoltaics community, and other applications such as semiconductor technology who are at the cutting edge of pilot-scale manufacture.Dermal denticles of thornback ray comprise of a dentine protrusion with an enamel cap. They were characterised with a correlative workflow for the first time, analysing the chemical, mechanical and microstructural properties to understand how the enamel layer can perform the required function. The correlative workflow for the dermal denticle consisted of optical microscopy, X-ray microtomography, scanning electron microscopy with energy dispersive X-ray spectroscopy, mechanical testing with nanoindentation, in-situ nanoindentation during X-ray microscopy along with computational modelling. The results show the potential function, of enamel as providing a sacrificial layer to protect the dentin body, it can do so with chemical enrichment, mechanically enhanced properties, and an optimised microstructure for wear resistance.This study demonstrates the application and development of correlative workflows for two different applications showcasing challenges and similarities. E-Thesis Swansea University Microscopy, workflows, X-ray CT, Electron microscopy, correlative workflows, carbon perovskite solar cells, biological functional layer 2 7 2025 2025-07-02 10.23889/SUThesis.71460 COLLEGE NANME COLLEGE CODE Swansea University Johnston, R., and Pleydell-Pearce, C. Doctoral EngD WEFO WEFO 2026-02-17T15:41:05.1915996 2026-02-17T15:23:44.1771432 Faculty of Science and Engineering School of Engineering and Applied Sciences - Materials Science and Engineering JEBIN JESTINE 1 71460__36252__380422a1927f4a36825d79c6430fe3a7.pdf 2024_Jestine_J.final.71460.pdf 2026-02-17T15:33:13.0883108 Output 134875307 application/pdf E-Thesis – open access true Copyright: the author, Jebin Jestine, 2026 true eng
title Linking microstructures and performances of functional coatings and engineering materials through multiscale and correlative microscopy methods
spellingShingle Linking microstructures and performances of functional coatings and engineering materials through multiscale and correlative microscopy methods
JEBIN JESTINE
title_short Linking microstructures and performances of functional coatings and engineering materials through multiscale and correlative microscopy methods
title_full Linking microstructures and performances of functional coatings and engineering materials through multiscale and correlative microscopy methods
title_fullStr Linking microstructures and performances of functional coatings and engineering materials through multiscale and correlative microscopy methods
title_full_unstemmed Linking microstructures and performances of functional coatings and engineering materials through multiscale and correlative microscopy methods
title_sort Linking microstructures and performances of functional coatings and engineering materials through multiscale and correlative microscopy methods
author_id_str_mv 760a6299a92c64d6d1650ebd6dcd9e4e
author_id_fullname_str_mv 760a6299a92c64d6d1650ebd6dcd9e4e_***_JEBIN JESTINE
author JEBIN JESTINE
author2 JEBIN JESTINE
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institution Swansea University
doi_str_mv 10.23889/SUThesis.71460
college_str Faculty of Science and Engineering
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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
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description Correlative characterisation workflows linking optical, electron and X-ray microscopy, enable researchers to chain multiple techniques, overcoming the limitations of any one technique. Applying correlative workflows create rich multimodal datasets covering chemical, mechanical and microstructural information across 2D and 3D, traversing length scales from macro to nanoscale. The application of correlative microscopy is becoming more common due to increased availability and improvements to techniques. Careful thought is required to prepare correlative workflows ensuring decisions do not have negative impacts on downstream processes e.g. destructive techniques should not limit further characterisation, if possible. For example, once a sample undergoes milling to prepare a cross section it is not possible to analyse the removed material.This study focusses on two specific applications/materials with differing origins, structures, chemistry and scale to demonstrate potential differences and similarities for users in very different fields. The two applications/materials are carbon-based perovskite solar cells, and thornback ray (Raja clavata) dermal denticle. The reason for selecting these two different materials is because they both have a thin functional layer which presents challenges for characterisation. The conductive layer of the carbon-based perovskite solar cell is around 20 microns, while the outer layer of the dermal denticle is around 30-50 microns.Carbon-based perovskite solar cells offer a low cost, efficient and stable design for photovoltaics. Within this EngD, these multilayered engineered devices have been characterised in 3D for the first time revealing the carbon flake orientations and porosity within the top mesoporous carbon layer and infiltration defects within the active layer. Three workflows of sample preparation and characterisation were designed and employed for these devices, and an optimised workflow was identified.With the carbon-based perovskite solar cell, the correlative workflow consisted of focused ion billing to prepare a pilar for X-ray microtomography, femtosecond laser machining for nano X-ray microscopy and focused ion beam tomography with energy dispersive X-ray spectroscopy. This work has the potential to become part of a feedback loop for researchers in the photovoltaics community, and other applications such as semiconductor technology who are at the cutting edge of pilot-scale manufacture.Dermal denticles of thornback ray comprise of a dentine protrusion with an enamel cap. They were characterised with a correlative workflow for the first time, analysing the chemical, mechanical and microstructural properties to understand how the enamel layer can perform the required function. The correlative workflow for the dermal denticle consisted of optical microscopy, X-ray microtomography, scanning electron microscopy with energy dispersive X-ray spectroscopy, mechanical testing with nanoindentation, in-situ nanoindentation during X-ray microscopy along with computational modelling. The results show the potential function, of enamel as providing a sacrificial layer to protect the dentin body, it can do so with chemical enrichment, mechanically enhanced properties, and an optimised microstructure for wear resistance.This study demonstrates the application and development of correlative workflows for two different applications showcasing challenges and similarities.
published_date 2025-07-02T05:38:41Z
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