Efficient, Scalable, and Solvent-free Mechanochemical Synthesis of the OLED Material Alq3 (q=8-Hydroxyquinolinate)
Efficient, Scalable, and Solvent-free Mechanochemical Synthesis of the OLED Material Alq3 (q=8-Hydroxyquinolinate)
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DOI：
10.1021/cg301291w
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发表时间：
2012-12-01
影响因子：
3.8
通讯作者：
James, Stuart L.
中科院分区：
文献类型：
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作者：
Ma, Xiaohe;Lim, Gin Keat;James, Stuart L.
以Al(OAc)(2)OH和8-羟基喹啉为原料，在无溶剂的机械力化学条件下，合成了在有机发光二极管材料中具有重要应用价值的铝配合物Alq(3)(Q=8-羟基喹啉)。机械力化学合成的初始产物是一种新型的Alq(3)的乙酸乙酸酯，随后对该相进行加热/解溶，得到Alq(3)的α晶型。机械化学法合成的AlQ(3)乙酸乙酸酯的结构已由粉末X射线衍射数据直接确定，其结构与AlQ(3)由醋酸溶液结晶得到的乙酸酯具有不同的晶型。值得注意的是，ALQ(3)的机械力化学合成被证明在从0.5到50克的两个数量级范围内完全可缩放。无溶剂机械力化学合成的Alq(3)样品分析纯，其发光行为与传统合成方法制备的样品相同。
The aluminum complex Alq(3) (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)(2)OH and 8-hydroxyquinoline by ball milling. The initial product of the mechanochemical synthesis is a novel acetic acid solvate of Alq(3), and the alpha polymorph of Alq(3) is obtained on subsequent heating/desolvation of this phase. The structure of the mechanochemically prepared acetic acid solvate of Alq(3) 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 Alq(3) from acetic acid. Significantly, the mechanochemical synthesis of Alq(3) is shown to be fully scalable across two orders of magnitude from 0.5 to 50 g scale. The Alq(3) 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.