Mechanochemical synthesis and crystal structure of a'-AlD 3 and a-AlD3

Brinks, H.W. , Istad-Lem, A. , Hauback, B.C.
Journal of physical chemistry B. - Vol. 110 (2006), no. 51, 25833-25837
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AlD3 was synthesized by ball milling of 3LiAlD4 + AlCl3. Planetary ball milling at room temperature resulted in a mixture of AlD3 (α and α′) and Al in addition to LiCl, whereas cryomilling at 77 K resulted in only AlD3 and LiCl. The AlD3 obtained was a mixture of about 2/3α and 1/3α′. α′ was determined by powder neutron diffraction to take the β-AlF3 structure with space group Cmcm and a = 6.470(3), b = 11.117(5), and c = 6.562(2) Å. It is built up of corner-sharing AlD6 octahedra in an open structure with hexagonal holes of radius 3.9 Å. α′ slowly decomposes during storage at 40°C. α-AlD3 is also described by a corner-sharing AlD 6 network but in a more dense ReO3-type arrangement. Both AlD3 modifications have slightly shorter Al-D distances compared to Na3AlD6, Na2LiAlD6, and K 2NaAlH6. © 2006 American Chemical Society.
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