[Perfluorosulfonate ionomer]/[SiO2-TiO2] nanocomposites via polymer-in situ sol-gel chemistry: Sequential alkoxide procedure
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Abstract:
In situ sol-gel chemistry was used to create inorganic/perfluoro-organic hybrids wherein titanium oxide outer regions of SiO2[1—x/4](OH)x nanoparticles, which were preformed in Nafion® membranes, were created by postreaction with tetrabutyltitanate (TBT). U-shaped Si and Ti distributions across the membrane thickness direction were determined via x-ray energy dispersive spectroscopy. Ti/Si ratio profiles are also U-shaped, indicating more Ti relative to Si in near-surface regions. IR spectroscopy verified structural bonding of TiO4 units onto SiO2 nanoparticles and indicated that alkoxide hydrolysis is not complete. Reacted silicon oxide nanophases retain the topological unconnectedness possessed by the corresponding unreacted phase. IR bands signifying molecular loops and linear fragments of Si(SINGLE BOND)O(SINGLE BOND)Si groups are seen. 29Si solid-state NMR spectroscopy indicated that, for an inorganic uptake of 16.3 wt %, the Q3 state of SiO4 is most populated although Q4 is only slightly less prominent and Q2 and Q1 are either small or absent. The silicon oxide component, although not being predominantly linear, retains a measure of uncondensed SiOH groups. Tensile stress vs. strain analyses suggested that TBT postreaction links nanoparticles, causing them to be contiguous over considerable distances. This percolative intergrowth occurs in near-surface regions generating a glassy zone. © 1996 John Wiley & Sons, Inc.Keywords:
Alkoxide
Ionomer
Nafion
Hybrid material
In situ sol-gel chemistry was used to create inorganic/perfluoro-organic hybrids wherein titanium oxide outer regions of SiO2[1—x/4](OH)x nanoparticles, which were preformed in Nafion® membranes, were created by postreaction with tetrabutyltitanate (TBT). U-shaped Si and Ti distributions across the membrane thickness direction were determined via x-ray energy dispersive spectroscopy. Ti/Si ratio profiles are also U-shaped, indicating more Ti relative to Si in near-surface regions. IR spectroscopy verified structural bonding of TiO4 units onto SiO2 nanoparticles and indicated that alkoxide hydrolysis is not complete. Reacted silicon oxide nanophases retain the topological unconnectedness possessed by the corresponding unreacted phase. IR bands signifying molecular loops and linear fragments of Si(SINGLE BOND)O(SINGLE BOND)Si groups are seen. 29Si solid-state NMR spectroscopy indicated that, for an inorganic uptake of 16.3 wt %, the Q3 state of SiO4 is most populated although Q4 is only slightly less prominent and Q2 and Q1 are either small or absent. The silicon oxide component, although not being predominantly linear, retains a measure of uncondensed SiOH groups. Tensile stress vs. strain analyses suggested that TBT postreaction links nanoparticles, causing them to be contiguous over considerable distances. This percolative intergrowth occurs in near-surface regions generating a glassy zone. © 1996 John Wiley & Sons, Inc.
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