Efficient, Scalable, and Solvent-free Mechanochemical Synthesis of the OLED Material Alq3 (q = 8-Hydroxyquinolinate)

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• 作者：Xiaohe Ma ; Gin Keat Lim ; Kenneth D. M. Harris ; David C. Apperley ; Peter N. Horton ; Michael B. Hursthouse ; Stuart L. James
• 刊名：Crystal Growth & Design
• 出版年：2012
• 出版时间：December 5, 2012
• 年：2012
• 卷：12
• 期：12
• 页码：5869-5872
• 全文大小：256K
• 年卷期：v.12,no.12(December 5, 2012)
• ISSN：1528-7505

文摘

The aluminum complex Alq₃ (q = 8-hydroxyquinolinate), which has important applications in organic light-emitting diode materials, is shown to be readily synthesized as a pure phase under solvent-free mechanochemical conditions from Al(OAc)₂OH and 8-hydroxyquinoline by ball milling. The initial product of the mechanochemical synthesis is a novel acetic acid solvate of Alq₃, and the 伪 polymorph of Alq₃ is obtained on subsequent heating/desolvation of this phase. The structure of the mechanochemically prepared acetic acid solvate of Alq₃ has been determined directly from powder X-ray diffraction data and is shown to be a different polymorph from the corresponding acetic acid solvate prepared by solution-state crystallization of Alq₃ from acetic acid. Significantly, the mechanochemical synthesis of Alq₃ is shown to be fully scalable across two orders of magnitude from 0.5 to 50 g scale. The Alq₃ sample obtained from the solvent-free mechanochemical synthesis is analytically pure and exhibits identical photoluminescence behavior to that of a sample prepared by the conventional synthetic route.