Optimising confocal Raman microscopy for spectral mapping of cement-based materials

Abstract

AbstractRaman 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.