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Updated: Jan 24, 2026

Structural Studies of Macromolecules in Solution using Small Angle X-Ray Scattering
Published on: November 5, 2018
In-Situ Angstrom-to-Micrometer Characterization of the Structural and Microstructural Changes in Kaolinite on Heating
Greeshma Gadikota1, Fan Zhang2, Andrew Allen2
1Department of Civil and Environmental Engineering, University of Wisconsin, Madison, WI 53706.
Abstract:
Synchrotron-based in-operando multi-scale X-ray scattering analyses are used to connect microstructural changes to phase changes in kaolinite on heating from 30 °C to 1150 °C. Combined ultra-small-angle and small-angle X-ray scattering (USAXS and SAXS) data are modeled to determine the hierarchical morphology of kaolinite comprising nano-scale interlayer pores, meso-scale pores, and larger interparticle voids, while wide-angle X-ray scattering (WAXS) data reveal the simultaneous evolution of molecular phases in kaolinite. We found that the transformation of kaolinite to metakaolin corresponds to the disappearance of nano-scale porosity, and the onset of sintered phases such as mullite consistent with the overall reduction in porosity. The emergence of nanoscale particulate features on heating above 900 °C corresponds to the onset of sintered phases such as spinel and mullite. This study illustrates the application of multi-scale X-ray scattering measurements to connect the thermally induced phase changes with changes in pore structure and fine morphology evolution.
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