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Silk is a protein-based natural polymer that has attracted considerable attention in recent research due to its outstanding mechanical properties and broad applications in biomedical research. This chapter presents an overview of NMR techniques used for elucidating the molecular structures and dynamics of silk, with a primary focus on silkworm silk, spider silk, and silk-mimic peptides. The rapid NMR technology development allows opportunities not only for characterizing structures of silk materials at high molecular/atomic resolution, but also for studying the silk protein dynamics and structural transition of silk protein in vivo and in vitro In this chapter, several recently developed NMR techniques along with classical techniques are discussed.

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