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X-ray diffraction: a powerful tool to probe and understand the structure of nanocrystalline calcium silicate hydrates

Abstract : X-ray diffraction (XRD) patterns were calculated and compared to literature data with the aim of investigating the crystal structure of nanocrystalline calcium silicate hydrates (C-S-H), the main binding phase in hydrated Portland cement pastes. Published XRD patterns from C-S-H of Ca/Si ratios ranging from similar to 0.6 to similar to 1.7 are fully compatible with nanocrystalline and turbostratic tobermorite. Even at a ratio close or slightly higher than that of jennite (Ca/Si = 1.5) this latter mineral, which is required in some models to describe the structure of C-S-H, is not detected in the experimental XRD patterns. The 001 basal reflection from C-S-H, positioned at similar to 13.5 angstrom when the C-S-H structural Ca/Si ratio is low (< 0.9), shifts towards smaller d values and sharpens with increasing Ca/Si ratio, to reach similar to 11.2 angstrom when the Ca/Si ratio is higher than 1.5. Calculations indicate that the sharpening of the 001 reflection may be related to a crystallite size along c* (i.e. a mean number of stacked layers) increasing with the C-S-H Ca/Si ratio. Such an increase would contribute to the observed shift of the 001 reflection, but fails to quantitatively explain it. It is proposed that the observed shift could result from interstratification of at least two tober-morite-like layers, one having a high and the other a low Ca/Si ratio with a basal spacing of 11.3 and 14 angstrom, respectively.
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Soumis le : mercredi 16 juillet 2014 - 12:25:22
Dernière modification le : lundi 25 juillet 2022 - 03:49:24

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Sylvain Grangeon, Francis Claret, Yannick Linard, Christophe Chiaberge. X-ray diffraction: a powerful tool to probe and understand the structure of nanocrystalline calcium silicate hydrates. Acta Crystallographica Section B : Structural Science [1968-2013], International Union of Crystallography, 2013, 69, pp.465-473. ⟨10.1107/S2052519213021155⟩. ⟨hal-01024545⟩



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