Nanoscale correlative X-ray spectroscopy and ptychography of carious dental enamel

This study reports the characterisation of human dental enamel caries using synchrotron nanoscale correlative ptychography and spectroscopic mapping in combination with scanning electron microscopy. A lamella ̴2.4 µm thick was extracted from a carious enamel region of a tooth using focused ion beam-...

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Main Authors: Cyril Besnard, Ali Marie, Sisini Sasidharan, Petr Buček, Jessica M. Walker, Julia E. Parker, Thomas E.J. Moxham, Benedikt Daurer, Burkhard Kaulich, Majid Kazemian, Richard M. Shelton, Gabriel Landini, Alexander M. Korsunsky
Format: Article
Language:English
Published: Elsevier 2022-12-01
Series:Materials & Design
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Online Access:http://www.sciencedirect.com/science/article/pii/S0264127522008942
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author Cyril Besnard
Ali Marie
Sisini Sasidharan
Petr Buček
Jessica M. Walker
Julia E. Parker
Thomas E.J. Moxham
Benedikt Daurer
Burkhard Kaulich
Majid Kazemian
Richard M. Shelton
Gabriel Landini
Alexander M. Korsunsky
author_facet Cyril Besnard
Ali Marie
Sisini Sasidharan
Petr Buček
Jessica M. Walker
Julia E. Parker
Thomas E.J. Moxham
Benedikt Daurer
Burkhard Kaulich
Majid Kazemian
Richard M. Shelton
Gabriel Landini
Alexander M. Korsunsky
author_sort Cyril Besnard
collection DOAJ
description This study reports the characterisation of human dental enamel caries using synchrotron nanoscale correlative ptychography and spectroscopic mapping in combination with scanning electron microscopy. A lamella ̴2.4 µm thick was extracted from a carious enamel region of a tooth using focused ion beam-scanning electron microscopy and transferred to two synchrotron beamlines to perform hard X-ray nano-fluorescence spectroscopy simultaneously with differential phase contrast mapping at a beam size of 55 × 45 nm. Soft X-ray ptychography data was then reconstructed with a pixel size of 8 nm. The two dimensional variation in chemistry and structure of carious enamel was revealed at the nanoscale, namely, the organisation of hydroxyapatite nano-crystals within enamel rods was imaged together with the inter-rod region. Correlative use of electron and X-ray scanning microscopies for the same sample allowed visualisation of the connection between structure and composition as presented in a compound image where colour indicates the relative calcium concentration in the sample, as indicated by the calcium Kα fluorescence intensity and grey scale shows the nanostructure. This highlights the importance of advanced correlative imaging to investigate the complex structure-composition relationships in nanomaterials of natural or artificial origin.
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spelling doaj.art-a1032d9a078c44cdb8613124c0d9a6e92022-12-22T03:02:04ZengElsevierMaterials & Design0264-12752022-12-01224111272Nanoscale correlative X-ray spectroscopy and ptychography of carious dental enamelCyril Besnard0Ali Marie1Sisini Sasidharan2Petr Buček3Jessica M. Walker4Julia E. Parker5Thomas E.J. Moxham6Benedikt Daurer7Burkhard Kaulich8Majid Kazemian9Richard M. Shelton10Gabriel Landini11Alexander M. Korsunsky12MBLEM, Department of Engineering Science, University of Oxford, Parks Road, Oxford, Oxfordshire OX1 3PJ, UK; Corresponding authors.MBLEM, Department of Engineering Science, University of Oxford, Parks Road, Oxford, Oxfordshire OX1 3PJ, UKMBLEM, Department of Engineering Science, University of Oxford, Parks Road, Oxford, Oxfordshire OX1 3PJ, UKTESCAN-UK Ltd., Wellbrook Court, Girton, Cambridge CB3 0NA, UKDiamond Light Source Ltd., Didcot, Oxfordshire OX11 0DE, UKDiamond Light Source Ltd., Didcot, Oxfordshire OX11 0DE, UKMBLEM, Department of Engineering Science, University of Oxford, Parks Road, Oxford, Oxfordshire OX1 3PJ, UK; Diamond Light Source Ltd., Didcot, Oxfordshire OX11 0DE, UKDiamond Light Source Ltd., Didcot, Oxfordshire OX11 0DE, UKDiamond Light Source Ltd., Didcot, Oxfordshire OX11 0DE, UKDiamond Light Source Ltd., Didcot, Oxfordshire OX11 0DE, UKSchool of Dentistry, University of Birmingham, 5 Mill Pool Way, Edgbaston, Birmingham, West Midlands B5 7EG, UKSchool of Dentistry, University of Birmingham, 5 Mill Pool Way, Edgbaston, Birmingham, West Midlands B5 7EG, UKMBLEM, Department of Engineering Science, University of Oxford, Parks Road, Oxford, Oxfordshire OX1 3PJ, UK; Corresponding authors.This study reports the characterisation of human dental enamel caries using synchrotron nanoscale correlative ptychography and spectroscopic mapping in combination with scanning electron microscopy. A lamella ̴2.4 µm thick was extracted from a carious enamel region of a tooth using focused ion beam-scanning electron microscopy and transferred to two synchrotron beamlines to perform hard X-ray nano-fluorescence spectroscopy simultaneously with differential phase contrast mapping at a beam size of 55 × 45 nm. Soft X-ray ptychography data was then reconstructed with a pixel size of 8 nm. The two dimensional variation in chemistry and structure of carious enamel was revealed at the nanoscale, namely, the organisation of hydroxyapatite nano-crystals within enamel rods was imaged together with the inter-rod region. Correlative use of electron and X-ray scanning microscopies for the same sample allowed visualisation of the connection between structure and composition as presented in a compound image where colour indicates the relative calcium concentration in the sample, as indicated by the calcium Kα fluorescence intensity and grey scale shows the nanostructure. This highlights the importance of advanced correlative imaging to investigate the complex structure-composition relationships in nanomaterials of natural or artificial origin.http://www.sciencedirect.com/science/article/pii/S0264127522008942Human enamel cariesSynchrotron correlative nanoanalysisX-ray fluorescence spectroscopyX-ray differential phase contrastX-ray ptychographyFIB-SEM
spellingShingle Cyril Besnard
Ali Marie
Sisini Sasidharan
Petr Buček
Jessica M. Walker
Julia E. Parker
Thomas E.J. Moxham
Benedikt Daurer
Burkhard Kaulich
Majid Kazemian
Richard M. Shelton
Gabriel Landini
Alexander M. Korsunsky
Nanoscale correlative X-ray spectroscopy and ptychography of carious dental enamel
Materials & Design
Human enamel caries
Synchrotron correlative nanoanalysis
X-ray fluorescence spectroscopy
X-ray differential phase contrast
X-ray ptychography
FIB-SEM
title Nanoscale correlative X-ray spectroscopy and ptychography of carious dental enamel
title_full Nanoscale correlative X-ray spectroscopy and ptychography of carious dental enamel
title_fullStr Nanoscale correlative X-ray spectroscopy and ptychography of carious dental enamel
title_full_unstemmed Nanoscale correlative X-ray spectroscopy and ptychography of carious dental enamel
title_short Nanoscale correlative X-ray spectroscopy and ptychography of carious dental enamel
title_sort nanoscale correlative x ray spectroscopy and ptychography of carious dental enamel
topic Human enamel caries
Synchrotron correlative nanoanalysis
X-ray fluorescence spectroscopy
X-ray differential phase contrast
X-ray ptychography
FIB-SEM
url http://www.sciencedirect.com/science/article/pii/S0264127522008942
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