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• W809673019 abstract "Polymer-layered silicate (PLS) nanocomposites are often based on natural clays such as montmorillonite. In EPR and NMR studies of the surfactant layer that compatibilizes the silicate and the polymer, we found that the iron content in these natural clays is detrimental, as it broadens spectra and shortens relaxation times. The problem was overcome by using as a layered silicate iron-free and structurally well defined magadiite, which was synthesized by a hydrothermal method. The morphology of the magadiite and the extent of intercalation in melt-prepared polymer-organo-magadiite nanocomposites were characterized by scanning electron microscopy (SEM) and wide-angle x-ray scattering (WAXS) respectively. Among different types of polymers, those with carbonyl groups appear to intercalate more easily. With iron-free magadiite, polycaprolactone (PCL) was found to intercalate into both ammonium surfactant modified and phosphonium surfactant modified organomagadiites. By using site-specific nitroxide spin probes and applying CW EPR (Continuous Wave Electron Paramagnetic Resonance) and pulse EPR techniques the dynamics and spatial structure of surfactant layers in such nanocomposites, were studied. Static H Nuclear Magnetic Resonance (NMR) on specifically deuterated cationic surfactants was also applied to access surfactant motion on a complementary time scale (milliseconds to microseconds) compared to EPR (nanoseconds). By CW EPR and H NMR, fast motion of surfactant layers was found to be pronounced by intercalation of PCL while it diminishes in non-intercalated microcomposites with polystyrene (PS). The rotational correlation times τc and activation energies Ea reveal different regimes of reorientation of surfactant molecules with increasing temperature. The transition temperature between the regimes is related to Tg of PS in microcomposites and to the melting temperature Tm of PCL in nanocomposites. The iron-free magadiite leads to substantially longer electron spin relaxation times and thus allows for pulse EPR experiments such as four-pulse double electron electron resonance (DEER), electron spin echo envelope modulation (ESEEM) and electron nuclear double resonance (ENDOR) on spin-labeled and specifically deuterated surfactants. ENDOR results suggest a model of the surfactant layers with a well-defined middle layer. This model can explain the dilution effects caused by PCL and PS polymers in the hybrids. Comprehensive information from these techniques nicely complements information from conventional characterization techniques such XRD and TEM and provides a much more detailed picture of structure and dynamics of the surfactant layer in polymer-layered silicate nanocomposites." @default.
• W809673019 created "2016-06-24" @default.
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• W809673019 date "2007-01-22" @default.
• W809673019 modified "2023-09-23" @default.
• W809673019 title "Synthesis and characterization of structurally well-defined polymer-layered silicate nanocomposites" @default.
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