Chinese Journal of Magnetic Resonance ›› 2012, Vol. 29 ›› Issue (3): 307-338.

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Applications of Advanced Solid-State NMR Techniques in Studying  the Structure and Dynamics of Polymers

 ZHANG Rong-Chun, SUN Ping-Chuan   

  1. Key Laboratory of Functional Polymer Materials of Ministry of Education, School of Physics and College of Chemistry, Nankai University, Tianjin 300071, China
  • Received:2011-09-14 Revised:2011-12-19 Online:2012-09-05 Published:2012-09-05
  • Supported by:

    国家杰出青年科学基金资助项目(20825416).

Abstract:

With the advances in NMR theories and spectrometer hardware technology, NMR is playing an increasingly important role in studying multiscale structure and dynamics of polymers. In this paper, the newest developments in solid-state 1H and 13C NMR techniques and their applications in the studies of polymer structures and dynamics were reviewed. High-resolution solid-state 1H NMR techniques, such as multiple-pulse and fast magic angle spinning (MAS), have made it possible to determine the chemical structures of polymers and to detect the intra- and inter-polymer interactions effectively. Taking advantages of through-bond (J- coupling) and through-space (dipolar coupling) interactions, two dimensional heteronuclear correlation NMR experiments now can be used to resolve the microstructures of complex polymer chains. The recoupling techniques allow dipolar interactions and chemical shift anisotropy to be observed under MAS conditions, thus enabling simultaneous detection of high-resolution 1H or 13C signals and quasi-static anisotropic interactions.  The domain sizes and interphase thickness in multiphase polymers and miscibility in polymer blends can now be determined effectively using the dipolar filter techniques. In the dynamics studies, it is now possible to obtain information on local fast motions of a single bond and super-slow chain dynamics by efficient suppression of spin-diffusion among protons and recoupling of chemical shift anisotropy. In summary, the advanced solid-state NMR techniques have enabled detailed studies on polymer microstructure, phase separation and dynamic behavior at different time and length scales, and on the relationship between the microstructure and macroscopic properties of polymers.

Key words: solid-state NMR, polymer, structure, dynamics

CLC Number: