Abstract
Fast magic-angle spinning solid-state proton NMR has been used to study the structure and dynamics of poly(ethyl acrylate) in bulk and polymerized in a Vycor glass with 40 A pores. Bulk poly(ethyl acrylate) is a low-T g material, and high-resolution solid-state proton NMR spectra are observed at ambient temperature because the dipolar interactions are averaged by the combination of chain motion and fast magic-angle sample spinning. The spectrum of the poly(ethyl acrylate)/Vycor composite shows signals in addition to those of the polymer that are assigned to water and surface hydroxyl groups in the porous glass. Integration of the composite and bulk poly(ethyl acrylate) signals reveals that the volume fraction of polymer in the pores is 0.56 and that the polymer occupies the central 30 A in a 40 A pore. Spin diffusion studies demonstrate that filling of the poly(ethyl acrylate)/Vycor is incomplete, and a fraction of the water in the pores is isolated from the polymer. Multiple-quantum NMR studies reveal a large difference in chain dynamics between the bulk poly(ethyl acrylate) and the porous glass composite, and 2D wide line separation NMR shows that the polymer is restricted at the surface of the pores but has bulklike mobility in the center of the pore.
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