119Sn Magic Angle Spinning NMR of Nanocrystalline SnO2
Abstract:Nanocrystalline SnO2 samples of different grain sizes, prepared by inert gas condensation technique (IGCT) and chemical precipitation method and conforming to the tetragonal phase, have been studied by variable speed (3–10 kHz) 119Sn MAS NMR at 11.74 Tesla field. 119Sn solid-state NMR results show that the IGCT prepared samples have good crystallinity and phase purity compared to the samples prepared by the chemical method. The determination of 119Sn chemical shielding parameters (iso, Δ and ) from slow MAS spectra shows that the 119Sn isotropic chemical shift (iso) is strongly influenced at smaller grain sizes, attributable to the change in the O2− local symmetry for the surface 119Sn ions at smaller grain sizes. The observed line widths in MAS spectra are significantly larger than the life-time broadening due to spin–lattice (T1) and spin–spin (T2) relaxation. The 119Sn MAS NMR spectra are thus inhomogeneously broadened by a distribution of isotropic chemical shifts, the line broadening increasing with decrease in grain size.
Document Type: Research Article
Publication date: January 1, 2008
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