Abstract

The solid-state NMR techniques of cross polarization (CP), high power proton decoupling and magic angle sample spinning allow one to study the binding of coupling agents to silica surfaces, γ-mercaptopropyltrimethoxysilane (y -MPTS), γ-aminopropyltriethoxy-silane (γ-APS), γ-glycidoxypropyltrimethoxysilane (γ-GPS), γ-metha-cryloxypropyltrimethoxysilane (γ-MPS) and vinyltriethoxysilane (VTES) were the organosilanes utilized on high-surface-area silica. High resolution solid-state 13C NMR spectra were obtained for coupling agents adsorbed on silica surfaces and for the corresponding coupling agents condensed as bulk polymers. Chemical shifts and line widths of the resonances of the chemically modified silicas are compared to those resonances arising from the bulk organosilanes. The spectra confirm chemical binding of the coupling agent to the silica surface. A graphite-filled epoxy is characterized in terms of molecular motion. In this study 13C spin-lattice relaxation times in the rotating frame of reference (T1ρ) were obtained for the composite.

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