Crystallization of non solvated aluminum hydride from a diethyl ether-benzene mixed solvent was studied. The desolvation of AlH 3 •(Et 2 O) x etherate in solution and the crystalliza tion of α AlH 3 during polythermal heating of the solution occur only in the presence of ≥10 wt.% LiAlH 4 . The process is multistage, and the crystallization begins with the formation of the AlH 3 •0.25Et 2 O solvate, which recrystallizes in the solid phase into γ AlH 3 and then α AlH 3 . Four crystalline modifications of aluminum hydride were characterized by X ray diffraction and electron microscopy.
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