Structural Analysis of Hybrid Titania-Based Mesostructured Composites
- 16 June 2005
- journal article
- Published by American Chemical Society (ACS) in Journal of the American Chemical Society
- Vol. 127 (27), 9721-9730
- https://doi.org/10.1021/ja050753r
Abstract
High-optical-quality titania-based mesostructured films with cubic or 2D-hexagonal symmetry were fabricated by combining trifluoroacetate (TFA)-modified titanium precursors with amphiphilic triblock poly(ethylene oxide)−poly(propylene oxide)−poly(ethylene oxide) (PEO−PPO−PEO) copolymers. The distribution, dynamics, and local environments of the TFA-modified titania, PEO, and PPO components of the hybrid were investigated. IR/Raman spectroscopy, in situ small-angle X-ray scattering, and transmission electron microscopy studies indicate that TFA coordinates the titanium center and forms a stable complex that is subsequently organized by the block copolymer species into ordered mesostructures. Solid-state NMR 19F→1H cross-polarization, 13C{1H} two-dimensional heteronuclear correlation, and 1H relaxation techniques were used to determine that PEO is predominantly incorporated within the TFA-modified titania, and that PPO environments encompass both microphase separated regions and interfacial regions composed of mixed PPO and TFA-modified titania. NMR 19F multiple-quantum spin counting measurements suggest that −CF3 groups of the trifluoroacetate ligands do not form clusters but instead randomly distribute within the inorganic component of the hybrid.Keywords
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