Efficiency of the refocused 31P-29Si MAS-J-INEPT NMR experiment for the characterization of silicophosphate crystalline phases and amorphous gels

被引:47
作者
Coelho, C. [1 ]
Azais, T. [1 ]
Bonhomme-Coury, L. [1 ]
Laurent, G. [1 ]
Bonhomme, C. [1 ]
机构
[1] Univ Paris 06, Lab Chimie Mat Condensee Paris, UMR 7574, F-75005 Paris, France
关键词
D O I
10.1021/ic061964f
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
One- and two-dimensional refocused MAS-J-INEPT NMR experiments in the solid state (through-bond polarization transfer) involving the highly abundant P-31 spin and the rare Si-29 spin are described for the crystalline silicophosphate phase Si5O(PO4)(6) and complex mixtures of SiP2O7 polymorphs. The evaluation of the (2)J(P-O-Si) coupling constants for all Si-29 sites is obtained by the careful analysis of the INEPT build-up curves under fast MAS. The results are in agreement with the crystallographic data, taking into account the various J coupling paths. The efficiency of the experiment is demonstrated by its application to more complex systems such as silicophosphate amorphous gels (obtained by the sol-gel process).
引用
收藏
页码:1379 / 1387
页数:9
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