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2008
ACL
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C.Coelho, T.Azais, C.Bonhomme, L.Bonhomme-Coury, C.Boissière, G.Laurent, D.Massiot, 'Efficiency of dipolar and J-derived solid-state NMR techniques for a new pair of nuclei {31P,29Si}. Towards the characterization of Si-O-P mesoporous materials', C. R. Chim. 11 387-397 (2008) doi:10.1016/j.crci.2007.09.012
Solid-state NMR methods based on dipolar and J-derived experiments such as CP, MAS-J-HMQC and MAS-J-INEPT MAS have been developed in the frame of the {31P,29Si} spin pair. The potential of these techniques has been demonstrated using model compounds including crystalline silicophosphate phases (Si5O(PO4)6 and various SiP2O7 polymorphs). Spatial interactions as well as through-bond connectivities were established. Evaluation of isotropic 2 JP-O-Si coupling constants has been established by careful analysis of the HMQC and INEPT build-up curves under fast MAS. The efficiency of the 31P →29Si CP MAS experiment for the detailed characterization of Si-O-P mesoporous materials (at low temperature) was demonstrated. The incorporation of P atoms in the silica network has been proved unambiguously. Such materials could be appropriate for biocompatibility purposes.
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