Analysis of in vitro demineralised human enamel using multi-scale correlative optical and scanning electron microscopy, and high-resolution synchrotron wide-angle X-ray scattering

Research output: Contribution to journalArticlepeer-review

Standard

Analysis of in vitro demineralised human enamel using multi-scale correlative optical and scanning electron microscopy, and high-resolution synchrotron wide-angle X-ray scattering. / Besnard, Cyril; Harper, Robert A.; Salvati, Enrico; Moxham, Thomas E.j.; Romano Brandt, León; Landini, Gabriel; Shelton, Richard M.; Korsunsky, Alexander M.

In: Materials and Design, Vol. 206, 109739, 08.2021.

Research output: Contribution to journalArticlepeer-review

Harvard

APA

Vancouver

Author

Bibtex

@article{7d2400c8ce704be09d1080a083a22462,
title = "Analysis of in vitro demineralised human enamel using multi-scale correlative optical and scanning electron microscopy, and high-resolution synchrotron wide-angle X-ray scattering",
abstract = "Enamel caries is a highly prevalent worldwide disease that involves the demineralisation of the outer tooth structure. In this study, we report the analysis of artificially demineralised human enamel sections ({\textquoteleft}slices{\textquoteright}) etched using lactic acid (2% v/v) in comparison with healthy enamel using correlative techniques of optical and electron microscopy, as well as scanning diffraction. Demineralisation of the enamel was characterised at the micron to sub-micron scale. The structure of the healthy enamel was investigated using Focused Ion Beam - Scanning Electron Microscopy (FIB-SEM) and compared with an etched sample to reveal their structural differences. Additional chemical analysis using energy-dispersive X-ray spectroscopy (EDS) was performed and a decrease in the Ca/P atomic % ratio was found in etched samples in comparison with healthy enamel, suggesting greater loss of calcium compared with phosphorus. Synchrotron wide-angle X-ray scattering (WAXS) was performed on the samples to reveal the differences in the diffraction patterns before and after etching in terms of lattice structure and preferred orientation (texture). Texture maps were extracted from diffraction analysis at 500 nm spatial resolution. These maps were correlated with the dimension of the enamel structure. The multi-scale correlative approach provided insights into the demineralisation-induced enamel structure alteration at a resolution approaching 500 nm.",
keywords = "Enamel, Energy-dispersive X-ray spectroscopy, In vitro demineralisation, Scanning electron microscopy, Synchrotron, X-ray diffraction",
author = "Cyril Besnard and Harper, {Robert A.} and Enrico Salvati and Moxham, {Thomas E.j.} and {Romano Brandt}, Le{\'o}n and Gabriel Landini and Shelton, {Richard M.} and Korsunsky, {Alexander M.}",
note = "Funding Information: This work was funded by The Engineering and Physical Sciences Research Council (EPSRC) entitled “Tackling human dental caries by multi-modal correlative microscopy and multi-physics modelling” (EP/P005381/1). The access to Diamond Light Source was under the proposal MT21419-1. Thanks to Diamond Light Source and particularly the team of B16 Dr. Igor Dolbnya and Dr. Oliver Fox, for beamline support and Dr. Jacob Filik for his support with the DAWN software. Thanks to Dr. Jonathan D. James (School of Dentistry, University of Birmingham) for support with preparation of the samples and optical imaging. Thanks to Petr Bu{\v c}ek (Tescan, U.K.) for support with FIB-SEM and Dr. Marzena Tkaczyk (Laboratory for In-situ Microscopy & Analysis, University of Oxford, U.K.) for support with sample coating. Publisher Copyright: {\textcopyright} 2021 The Authors",
year = "2021",
month = aug,
doi = "10.1016/j.matdes.2021.109739",
language = "English",
volume = "206",
journal = "Materials and Design",
issn = "0264-1275",
publisher = "Elsevier",

}

RIS

TY - JOUR

T1 - Analysis of in vitro demineralised human enamel using multi-scale correlative optical and scanning electron microscopy, and high-resolution synchrotron wide-angle X-ray scattering

AU - Besnard, Cyril

AU - Harper, Robert A.

AU - Salvati, Enrico

AU - Moxham, Thomas E.j.

AU - Romano Brandt, León

AU - Landini, Gabriel

AU - Shelton, Richard M.

AU - Korsunsky, Alexander M.

N1 - Funding Information: This work was funded by The Engineering and Physical Sciences Research Council (EPSRC) entitled “Tackling human dental caries by multi-modal correlative microscopy and multi-physics modelling” (EP/P005381/1). The access to Diamond Light Source was under the proposal MT21419-1. Thanks to Diamond Light Source and particularly the team of B16 Dr. Igor Dolbnya and Dr. Oliver Fox, for beamline support and Dr. Jacob Filik for his support with the DAWN software. Thanks to Dr. Jonathan D. James (School of Dentistry, University of Birmingham) for support with preparation of the samples and optical imaging. Thanks to Petr Buček (Tescan, U.K.) for support with FIB-SEM and Dr. Marzena Tkaczyk (Laboratory for In-situ Microscopy & Analysis, University of Oxford, U.K.) for support with sample coating. Publisher Copyright: © 2021 The Authors

PY - 2021/8

Y1 - 2021/8

N2 - Enamel caries is a highly prevalent worldwide disease that involves the demineralisation of the outer tooth structure. In this study, we report the analysis of artificially demineralised human enamel sections (‘slices’) etched using lactic acid (2% v/v) in comparison with healthy enamel using correlative techniques of optical and electron microscopy, as well as scanning diffraction. Demineralisation of the enamel was characterised at the micron to sub-micron scale. The structure of the healthy enamel was investigated using Focused Ion Beam - Scanning Electron Microscopy (FIB-SEM) and compared with an etched sample to reveal their structural differences. Additional chemical analysis using energy-dispersive X-ray spectroscopy (EDS) was performed and a decrease in the Ca/P atomic % ratio was found in etched samples in comparison with healthy enamel, suggesting greater loss of calcium compared with phosphorus. Synchrotron wide-angle X-ray scattering (WAXS) was performed on the samples to reveal the differences in the diffraction patterns before and after etching in terms of lattice structure and preferred orientation (texture). Texture maps were extracted from diffraction analysis at 500 nm spatial resolution. These maps were correlated with the dimension of the enamel structure. The multi-scale correlative approach provided insights into the demineralisation-induced enamel structure alteration at a resolution approaching 500 nm.

AB - Enamel caries is a highly prevalent worldwide disease that involves the demineralisation of the outer tooth structure. In this study, we report the analysis of artificially demineralised human enamel sections (‘slices’) etched using lactic acid (2% v/v) in comparison with healthy enamel using correlative techniques of optical and electron microscopy, as well as scanning diffraction. Demineralisation of the enamel was characterised at the micron to sub-micron scale. The structure of the healthy enamel was investigated using Focused Ion Beam - Scanning Electron Microscopy (FIB-SEM) and compared with an etched sample to reveal their structural differences. Additional chemical analysis using energy-dispersive X-ray spectroscopy (EDS) was performed and a decrease in the Ca/P atomic % ratio was found in etched samples in comparison with healthy enamel, suggesting greater loss of calcium compared with phosphorus. Synchrotron wide-angle X-ray scattering (WAXS) was performed on the samples to reveal the differences in the diffraction patterns before and after etching in terms of lattice structure and preferred orientation (texture). Texture maps were extracted from diffraction analysis at 500 nm spatial resolution. These maps were correlated with the dimension of the enamel structure. The multi-scale correlative approach provided insights into the demineralisation-induced enamel structure alteration at a resolution approaching 500 nm.

KW - Enamel

KW - Energy-dispersive X-ray spectroscopy

KW - In vitro demineralisation

KW - Scanning electron microscopy

KW - Synchrotron

KW - X-ray diffraction

UR - http://www.scopus.com/inward/record.url?scp=85105270595&partnerID=8YFLogxK

U2 - 10.1016/j.matdes.2021.109739

DO - 10.1016/j.matdes.2021.109739

M3 - Article

VL - 206

JO - Materials and Design

JF - Materials and Design

SN - 0264-1275

M1 - 109739

ER -