Ilett, M, Freeman, HM orcid.org/0000-0001-8242-9561, Aslam, Z et al. (11 more authors) (2022) Evaluation of correlated studies using liquid cell and cryo-transmission electron microscopy: Hydration of calcium sulphate and the phase transformation pathways of bassanite to gypsum. Journal of Microscopy, 288 (3). pp. 155-168. ISSN 0022-2720
Abstract
Insight into the nucleation, growth and phase transformations of calcium sulfate could improve the performance of construction materials, reduce scaling in industrial processes and aid understanding of its formation in the natural environment. Recent studies have suggested that the calcium sulfate pseudo polymorph, gypsum (CaSO₄·2H₂O) can form in aqueous solution via a bassanite (CaSO₄·0.5H₂O) intermediate. Some in situ experimental work has also suggested that the transformation of bassanite to gypsum can occur through an oriented assembly mechanism. In this work, we have exploited liquid cell transmission electron microscopy (LCTEM) to study the transformation of bassanite to gypsum in an undersaturated aqueous solution of calcium sulfate. This was benchmarked against cryogenic TEM (cryo-TEM) studies to validate internally the data obtained from the two microscopy techniques. When coupled with Raman spectroscopy, the real-time data generated by LCTEM, and structural data obtained from cryo-TEM show that bassanite can transform to gypsum via more than one pathway, the predominant one being dissolution/reprecipitation. Comparisons between LCTEM and cryo-TEM also show that the transformation is slower within the confined region of the liquid cell as compared to a bulk solution. This work highlights the important role of a correlated microscopy approach for the study of dynamic processes such as crystallisation from solution if we are to extract true mechanistic understanding.
Metadata
Item Type: | Article |
---|---|
Authors/Creators: |
|
Copyright, Publisher and Additional Information: | © 2022 The Authors. Journal of Microscopy published by John Wiley & Sons Ltd on behalf of Royal Microscopical Society. This is an open access article under the terms of the Creative Commons Attribution License, which permits use, distribution and reproduction in any medium, provided the original work is properly cited. |
Keywords: | calcium sulphate; cryogenic TEM; crystallisation; liquid phase TEM |
Dates: |
|
Institution: | The University of Leeds |
Academic Units: | The University of Leeds > Faculty of Engineering & Physical Sciences (Leeds) > School of Chemical & Process Engineering (Leeds) The University of Leeds > Faculty of Engineering & Physical Sciences (Leeds) > School of Chemistry (Leeds) > Inorganic Chemistry (Leeds) The University of Leeds > Faculty of Engineering & Physical Sciences (Leeds) > School of Civil Engineering (Leeds) The University of Leeds > Faculty of Engineering & Physical Sciences (Leeds) > School of Physics and Astronomy (Leeds) > Condensed Matter (Leeds) The University of Leeds > Faculty of Biological Sciences (Leeds) > School of Biomedical Sciences (Leeds) |
Funding Information: | Funder Grant number EPSRC (Engineering and Physical Sciences Research Council) EP/R018820/1 EPSRC (Engineering and Physical Sciences Research Council) EP/P00122X/1 EPSRC (Engineering and Physical Sciences Research Council) EP/M028143/1 EPSRC (Engineering and Physical Sciences Research Council) EP/J021156/1 EPSRC (Engineering and Physical Sciences Research Council) EP/K00512X/1 |
Depositing User: | Symplectic Publications |
Date Deposited: | 08 Apr 2022 11:12 |
Last Modified: | 01 Feb 2023 02:06 |
Status: | Published |
Publisher: | Wiley |
Identification Number: | 10.1111/jmi.13102 |
Related URLs: | |
Open Archives Initiative ID (OAI ID): | oai:eprints.whiterose.ac.uk:185528 |