A comprehensive spectroscopic characterization of all known crystalline AlF3 phases (??-, ??-, ??-, ??-, ??-AlF3) is presented for the first time in this study. Beside their X-ray diffraction powder patterns, which were already published in the literature, 27Al and 19F MAS NMR, FT IR and XPS spectroscopic techniques were applied for all phases in a consistent manner. For all phases prepared the utilization of 27Al satellite transition (SATRAS) NMR allowed to determine the quadrupolar parameters of the aluminium sites including their distributions. In addition, ??-AlF3 was isolated with high phase purity and characterized following a new preparation path different from those known so far in the literature. ?? 2009 Elsevier B.V. All rights reserved.
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