Abstract
In-situ energy dispersive X-ray diffractometry (EDXRD) using synchrotron radiation has been used to directly observe the kinetics of formation of a geopolymeric gel from a metakaolin precursor. The use of a purpose-built hydrothermal cell with polychromatic radiation from a wiggler source enables collection of a full diffraction pattern approximately every 150 s. This provides sufficient time resolution to observe the collapse of the metakaolin structure as it dissolves in the activating solution, accompanied by the reprecipitation of the geopolymeric gel binder phase from the now-supersaturated solution. Measurements taken on a limited set of samples of different composition (Si/Al ratio) show a clear trend in the rate of reaction with composition, and also a distinctly different mechanism of reaction in the most highly alkaline systems compared to those containing higher levels of dissolved silica in the activating solution. This corresponds to the results of previous microscopic observations showing significantly different microstructures in these systems, and confirms the value of this technique in analysis of the kinetics of geopolymerisation.
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Acknowledgements
The experimental portion of this work was carried out on beamline X17C at the National Synchrotron Light Source, Brookhaven National Laboratory, which is supported by the U.S. Department of Energy under Contract No. DE AC02-98CH10886. Valuable technical assistance from Dr. Jingzhu Hu is gratefully acknowledged. This work was funded through the Particulate Fluids Processing Centre, a Special Research Centre of the Australian Research Council, and by an Australian-American Fulbright Postgraduate Scholarship awarded to JLP and hosted by the University of Illinois at Urbana-Champaign and the University of Delaware.
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Provis, J.L., van Deventer, J.S.J. Direct measurement of the kinetics of geopolymerisation by in-situ energy dispersive X-ray diffractometry. J Mater Sci 42, 2974–2981 (2007). https://doi.org/10.1007/s10853-006-0548-z
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DOI: https://doi.org/10.1007/s10853-006-0548-z