A novel triblock copolymer containing azobenzene (AZO) and N-isopropylacrylamide (NIPAM) was synthesized by atom transfer radical polymerization (ATRP) using a poly(ethylene oxide) bifunctional macroinitiator (Br-PEO-Br). The triblock copolymer was characterized by 1H NMR and gel permeation chromatography (GPC). Uniformly distributed polymeric micelles were obtained in aqueous solution by self-assembly method. Transmission electron microscope (TEM), fluorescence spectroscopy and dynamic light scattering (DLS) were used for the investigation of the self-assemblies and their stimuli-responsive behavior. Photoinduced release behavior was achieved with the as-prepared triblock copolymer micelles, which has not been observed in our previously-reported diblock copolymer micelles: the fluorescence intensity of Nile Red trapped in the triblock copolymer micelles dropped by approximately 40% after UV and Vis light alternative irradiation, indicating that a portion of the Nile Red was released to the aqueous media. Besides, the micelles shrank during the heating process.
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