Optimising confocal Raman microscopy for spectral mapping of cement-based materials
File(s)Zhang2022_Article_OptimisingConfocalRamanMicrosc.pdf (2.63 MB)
Published version
Author(s)
Zhang, Kai
Yio, M
Wong, Hong
Buenfeld, N
Type
Journal Article
Abstract
Raman spectroscopy combined with confocal imaging, i.e. confocal Raman microscopy (CRM) is a relatively new technique with huge potential for high-resolution chemical mapping of phase composition and spatial distribution in cement-based materials. However, the effects of sample preparation and various operating parameters on mapping quality has not been systematically studied. This paper optimises CRM for spectral mapping of carbonated and non-carbonated cement-based materials. The effects of sample preparation and scanning parameters on the detection of four main phases (calcite, portlandite, ettringite and unreacted cement) were investigated. Results show that although freshly cut cementitious samples can be analysed as-is, the Raman signals improve with short gentle drying and surface grinding/polishing prior to analysis. Increasing laser power, exposure time and scan accumulation, and short laser wavelength yields higher signal-to-noise (SNR) ratio in the obtained spectrum. The use of a 4.15 mW laser power, 2 s exposure time and scan accumulation of 2 with 532 nm laser represents a good operating condition for Raman analysis of cement-based materials. This produces SNR > 10 for all investigated phases at short testing time and low risk of laser-induced damage. Microcracking caused by localised heating during closely-spaced mapping can be limited by impregnating the sample with epoxy to protect the microstructure. We show for the first time that CRM can be used to quantify the volume fraction of calcium carbonate and portlandite at high resolution when combined with SEM. The advantages and limitations of CRM for mapping cement-based materials are discussed.
Date Issued
2022-05-14
Date Acceptance
2022-05-01
Citation
Materials and Structures, 2022, 55 (131), pp.1-18
ISSN
1359-5997
Publisher
Springer
Start Page
1
End Page
18
Journal / Book Title
Materials and Structures
Volume
55
Issue
131
Copyright Statement
© 2022 The Author(s). Open Access This article is licensed under a Creative Commons Attribution 4.0 International License, which permits use, sharing, adaptation, distribution and reproduction in any medium or format, as long as you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons licence, and indicate if changes were made. The images or other third party material in this article are included in the article's Creative Commons licence, unless indicated otherwise in a credit line to the material. If material is not included in the article's Creative Commons licence and your intended use is not permitted by statutory regulation or exceeds the permitted use, you will need to obtain permission directly from the copyright holder. To view a copy of this licence, visit http://creativecommons.org/licenses/by/4.0/.
License URL
Identifier
https://link.springer.com/article/10.1617/s11527-022-01979-9
Subjects
Building & Construction
0905 Civil Engineering
Publication Status
Published
Date Publish Online
2022-05-14