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Calcium silicate hydrate—in-situ development of the silicate structure followed by infrared spectroscopy

John, Elisabeth; Stephan, Dietmar

In the current study, the development of the silicate structure of synthetic calcium silicate hydrates with different calcium contents was followed by in-situ infrared (IR) spectroscopy and correlated to the in-situ phase development evaluated by X-ray diffraction (XRD). A baseline correction method initially developed for X-ray diffractograms was successfully adapted for the complex background of the fingerprint region in in-situ IR, which significantly contributed to signal quality and reproducibility. The development of separate silicate infrared bands could be monitored over 24 h of reaction. These bands could be assigned to oligomeric and dimeric species based on their time and stoichiometry-dependent development. It was clearly shown that the main peak of the dimeric silicate species was overlooked in the literature. The correlation of time-dependent events to in-situ XRD revealed that changes in the unit cell of calcium silicate hydrate are related to silicate polymerization. The results were compared to 29Si-MAS-NMR, which highlighted the benefits of in-situ IR spectroscopy.
Published in: Journal of the American Ceramic Society, 10.1111/jace.18019, Wiley