REVERSIBLE DISSOCIATION AND FORMATION OF AZOBENZENE BLOCK COPOLYMER MICELLES in Java

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6.4. REVERSIBLE DISSOCIATION AND FORMATION OF AZOBENZENE BLOCK COPOLYMER MICELLES
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The block copolymer of P(tBA-co-AA)-b-PAzoMA can form core shell micelles and vesicles depending on the composition and the preparation conditions (Tong et al., 2005; Wang et al., 2004). With the same length of the hydrophobic block of PAzoMA, the actual hydrolysis degree of tBA on the hydrophilic P(tBA-co-AA) random copolymer turns out to be important since it determines the hydrophilic
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CHAPTER 6: AZOBENZENE CONTAINING BLOCK COPOLYMER MICELLES
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hydrophobic balance. At some block copolymer compositions, the micellar aggregates respond to light exposure in a sensitive way and display clearly reversible dissociation and reformation upon alternating UV and visible light irradiation that switches the dipole moment of azobenzene pendant groups and thus the entire polarity of the PAzoMA block. Unless otherwise stated, the results obtained with the sample of P(tBA46-co-AA22)-b-PAzoMA74 are used for discussion, with micellar aggregates prepared using the method developed for amphiphilic BCPs that are not soluble in water. The method consists in rst dissolving the BCP in a good organic solvent for both blocks and then adding slowly a certain amount of water with which the organic solvent is miscible, to trigger the aggregation of the hydrophobic polymer chains in the mixed solvent to form the core of micelle or the membrane of vesicle (Fig. 6.1). Usually, a large volume of water (e.g., 10-fold) is subsequently added to quench the micellar aggregates thus formed. In case an aqueous micellar solution is needed, the organic solvent can be removed either by evaporation or through dialysis against water. Figure 6.3 shows the scanning electron microscope (SEM) images of a core shell micellar solution before UV, after UV and after subsequent visible light irradiation (all solutions were cast on a silicon wafer and dried prior to the SEM observation). Core shell micelles with diameters around 15 nm were formed in the initial solution; after exposure of the solution to UV light (360 nm, 35 mW cm 2), most micelles were disappeared. However, when this UV irradiated solution was subsequently exposed to visible light (440 nm, 39 mW cm 2), micelles reappeared in the cast sample. This observation clearly shows the reversible dissociation and formation of core shell micelles of P(tBA46-co-AA22)-b-PAzoMA74 as a result of the trans cis photoisomerization of azobenzene groups on PAzoMA. The same conclusion was also reached for larger vesicles of this BCP (diameter B200 nm) that can be formed by adding more water into the dioxane BCP solution. In addition to SEM observations, the larger micellar aggregates in solution scatter more light, which makes possible the in situ monitoring of the
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Figure 6.3. SEM images of core-shell micelles of P(tBA46-co-AA22)-b-PAzoMA74 formed by adding 9%, in volume, of water in dioxane solution with initial polymer concentration of 1 mg mL 1: before irradiation, after UV and visible light irradiation. Source: Wang et al., 2004. Reprinted with permission.
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6.4. REVERSIBLE DISSOCIATION AND FORMATION OF AZOBENZENE
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kinetic processes of light-induced dissociation and formation of the vesicles through measurements of the transmittance of a probe light (a He Ne laser at 633 nm) whose wavelength is far from the absorption of the chromophore. An example of results is given in Fig. 6.4. In this speci c case, the vesicular solution was prepared by adding 16% of water (v/v) in a dioxane solution of P(tBA46-coAA22)-b-PAzoMA74 (1 mg mL 1). When UV light (360 nm, 18 mW cm 2) was applied vertically from the top of the cuvette, in which was placed the vesicular solution (B1.5 mL) under stirring, the optical transmittance increased quickly
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2 m 10.5 10.0 9.5 9.0 8.5 8.0 C 7.5 7.0 10 0 10 20 30 40 50 60 70 80 90 100 110 120 Time (s) A UV-on B Visible-on
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Figure 6.4. Changes in transmittance for a vesicle solution of P(tBA46-co-AA22)-bPAzoMA74 exposed to UV (360 nm, 18 mW cm 2) and visible (440 nm, 24 mW cm 2) light irradiation, vesicles being formed by adding 16%, in volume, of water in a dioxane solution with initial polymer concentration of 1 mg mL 1. Typical SEM images for samples cast from the solution at different times indicated in the gure show the vesicles before irradiation, their dissociation by UV irradiation and reformation by visible irradiation. For comparison, also shown is the transmittance of the dioxane solution (no water added to induce the aggregation of the polymer) subjected to the same conditions of UV and visible light irradiation. Source: Tong et al., 2005. Reprinted with permission.
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