Order and disorder in Titanosilicate glass by 17O MAS, off-MAS and 3Q-QCPMG-MAS solid state NMR

Abstract : An 17O-enriched version of the titanosilicate glass, KTS2 (K2O‚TiO2‚2SiO2), was analyzed by 17O MAS, off-MAS, and 3Q-QCPMG-MAS experiments. Exploiting the variations in EFG and CSA parameters for the 17O sites in KTS2 glass, we detected four types of oxygen by reduction of spinning sideband intensities in the off-MAS experiments. From the 17O off-MAS and 3Q-QCPMG-MAS experiments, the Si-O-Ti and K-O- Ti resonances were characterized by a distribution of isotropic chemical shifts, whereas the Si-O-Si resonance was characterized by very small distributions of both EFG tensor and isotropic chemical shift, which means that the disorder in the glass is closely related to Ti. In addition to the order/disorder issue, the most striking feature about the 17O off-MAS experiments on KTS2 is the lack of signals from Ti-O-Ti, which contradicts linking between corner sharing TiO5 units. Therefore, the structure must consist of linkages between TiO5 units and SiO4 tetrahedra and linkages between SiO4 tetrahedra.
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F. Larsen, Stéphanie Rossano, I. Farnan. Order and disorder in Titanosilicate glass by 17O MAS, off-MAS and 3Q-QCPMG-MAS solid state NMR. Journal of Physical Chemistry B, American Chemical Society, 2007, 111 (28), pp.8014-8019. ⟨hal-00725689⟩

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