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Ordered nonlamellar mesoporous aluminophosphates and galloaluminophosphates have been synthesized by introducing phosphate linking groups to cluster/surfactants salts of prearranged AlO4Al12(OH)24(H2O)12 7+ (Al13) and GaO4Al12(OH)24(H2O)12 7+ (GaAl12) tridecamers. The Al13 and GaAl12 polyoxocations form a layered mesoscopic salt with the anionic surfactant sodium dodecylsulfate. Upon the reaction with a buffered hydrogen phosphate/dihydrogen phosphate solution the layers of clusters are transformed into a nonlayered, nearly hexagonal mesoscopic phase. Removal of the surfactant from the alumino- and galloaluminophosphates by anion-exchange results in mesoporous materials with BET surface areas up to 630 and 455 m2/g, respectively. FT-IR and 27Al and 31P MAS−NMR as well as 27Al → 31P cross-polarization experiments indicate that the phosphate treatment results in the formation of new bonds between aluminate and phosphate species. A fraction of the clusters are transformed leading to an increase in the number of tetrahedral aluminate groups in the product. Multiple anion-exchange, e.g., with acetate, dichromate, or naphthol yellow S ions, is possible in these open mesoporous structures, which form a new class of inorganic anion-exchangers.

Variable-temperature (VT) solid-state 19 F NMR spectroscopy with high-speed magic-angle spinning (MAS) has been used to study copolymers of vinylidene fluoride and hexafluoropropylene and of vinylidene fluoride and chlorotrifluoroethylene, and terpolymers of vinylidene fluoride, tetrafluoroethylene, and hexafluoropropylene. High-resolution spectra were obtained by simultaneously using MAS speeds up to 25 kHz and heating to 250°C. Sufficient resolution was achieved to assign peaks by comparison to results obtained from solution-state NMR studies and to determine the monomer composition of the polymer.

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