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Herein, we reported on the precise growth and optical waveguide characteristics of hexagonal tris(8-hydroxyquinoline)aluminum(Ⅲ) (Alq₃) micro-crystals (MCs). The hexagonal Alq₃ MCs were prepared using surfactant-assisted assembly growth with the help of cetyltrimethylammoniumbromide (CTAB), in which the crystallization occurred as a result of molecular assembly and packing. Also, we adjusted the molar ratio of Alq₃ and CTAB for the control degree of crystallization. The formation and structure of Alq₃ MCs were investigated using field-emission scanning electron microscopy and X-ray diffraction pattern experiments, respectively. The solid-state laser confocal microscope-photoluminescence spectra and charge-coupled device images for the Alq₃ MCs were measured to study the luminescence efficiency and colors, respectively. The optical waveguide performance of the hexagonal Alq₃ MCs was measured for each side direction. According to our results, crystalline Alq₃ micro-crystals are promising materials for application to the development of optical communication devices.