NMR Methodologies for the Detection and Quantification of Nanostructural Defects in Silicone Networks

We present and discuss a sensitive spectroscopic means of detecting and quantifying network defects within a series of polysiloxane elastomers through a novel application of 19F solution state nuclear magnetic resonance (NMR). Polysiloxanes are the most utilized non-carbon polymeric material today....

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Bibliographic Details
Published in:Macromolecules 2018-03, Vol.51 (5), p.1992-2001
Main Authors: Rodriguez, Jennifer N, Alviso, Cynthia T, Fox, Christina A, Maxwell, Robert S, Lewicki, James P
Format: Article
Language:English
Subjects:
INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
MATERIALS SCIENCE
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Summary:We present and discuss a sensitive spectroscopic means of detecting and quantifying network defects within a series of polysiloxane elastomers through a novel application of 19F solution state nuclear magnetic resonance (NMR). Polysiloxanes are the most utilized non-carbon polymeric material today. Their final network structure is complex, hierarchical, and often ill-defined due to modification. Characterization of these materials with respect to starting and age-dependent network structure is obfuscated by the intractable nature of polysiloxane network elastomers. We report a synthetic strategy for selectively tagging chain-end silanols with an organofluorine compound, which may then be conveniently and quantitatively measured as a function of structure and environment by means of 19F NMR. This study represents a new and sensitive means of directly quantifying aspects of network architecture in polysiloxane materials and has the potential to be a powerful new tool for the spectroscopic assessment of structural dynamic response in polysiloxane networks.
ISSN:0024-9297
1520-5835
DOI:10.1021/acs.macromol.7b02197