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7.2.3. Associative Phase Separation
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Finally, other type of phase separation can help achieving marked macroscopic ampli cation upon crossing a critical condition of demixing. In addition to LCST properties, water-soluble polymer can also be made abruptly insoluble upon association with nanoparticles, such as a protein and micelles of surfactants (Piculell and Lindman, 1992). Owing to their importance for industrial products (cosmetic, food, personal care), polymer surfactant demixings have been extensively studied. Making these system responsive to light would open a vast range of applications. Two classes of phase separation have to be distinguished, namely, seggregative (formation of a surfactant-rich phase and a polymer-rich one, when the two partners have no propensity to bind) and associative separation (demixing of a dense phase containing associates of surfactant and polymer). Here we are interested in the associative separation because photoisomerization could signi cantly affect the association strength. Basically, the association with nanoparticles can evolve enough energy to balance the translation entropies of both the chains and particles. In turn, phase separation (sometimes called coacervation) occurs between a concentrated phase maximizing the particle/polymer contacts and a very dilute phase, possibly containing the excess of unbound nanoparticles or almost particle-free polymer chains. At variance with the chains showing LCST behavior, the demixing can be obtained in good solvent for the bare polymer. These important distinctions lead to phase separation at low temperature and homogeneity at high temperature (upper critical solubility, UCST), as shown in Fig. 7.4a. This type of nonresponsive phase separation has been commonly achieved by hydrophobic association of charged polymers and neutral surfactants (hydrophobe containing polyelectrolytes are more easily water-soluble than neutral amphiphilic chains) (Iliopoulos, 1998; Piculell and Lindman, 1992). It is also possible to use neutral polymer in combination with ionic micelles. When one partner is ionic, however, the contribution of counter-ion to the translational entropy must be reduced to afford the formation of a concentrated, ion-containing phase. The presence of simple salt (e.g., NaCl) at concentrations above 100 mM is usually suf cient to enlarge the two-phase region in the phase map (Howley et al., 1997; Ef ng et al., 1994). Because the E to Z photoswitch decreases the propensity of an azo-modi ed chain to bind to apolar domains, such as the core of micelles, the UCST of mixed surfactant/azobenzene-modi ed polymers (AMP) is expected and actually shown to decrease upon UV exposure. Temperature drops by 101C 151C have been reported (Howley et al., 1997). When the system is investigated in the temperaturewindow between UCST (UV) and UCST (dark), the phase diagram displays a large biphasic surface for the dark-adapted system, whereas the biphasic domain disappears completely under UV exposure. Fig. 7.4b illustrates the case of an azobenzene-modi ed polyacrylate mixed with dodecylPEO surfactant (C12E4). At room temperature, solutions well above the CMC of C12E4 were supplemented with increasing amount of polymer. Because of the low density of the surfactant, the C12E4-rich phase formed in the dark with small quantities of
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polymer was creaming, whereas the phase formed in the presence of higher polymer concentrations was denser and sedimented. Exposure to UV light made all mixtures homogeneous, and a single phase can be seen after centrifugation, irrespective of the composition. In addition, the range of temperature affording photoresponsiveness is much larger than just the UCST differences between UV and blue exposed (or dark-adapted) samples. Provided that the composition of sample can be adjusted, responsiveness would be found at almost all temperature below UCST (dark). The plot in Fig. 7.4a shows how the downshift of the twophase region creates a long strip between the dark and UV-adapted boundaries in the (temperature vs. surfactant) diagram. At any temperature lower than UCST (UV), it is possible to shift the composition toward the left-hand side of the diagram (increase of the surfactant concentration slightly above the UV-adapted phase separation point) to bring the system to an homogeneous state under UV exposure that turns into a two-phase system in the dark (Fig. 7.4c) (Howley et al., 1997; Ef ng and Kwak, 1995). Basically, the attractive contribution that causes the phase separation comes down to the sharing of one nanoparticle between two or more segments of polymer chains. The particles act as transient cross-links, which are somehow equivalent to interchain attraction. In semidilute solution, the number of such interchain cross-links could exceed the initial number of interpolymer contacts if the concentration of particles is increased above a critical threshold. This leads to a decrease of the correlation length above this critical concentration of cross-linker, and in turn to the shrinkage of the network (also called syneresis). Following Leibler and colleagues (Pezron et al., 1988; Keita et al., 1995), the onset of phase separation corresponds to the exact matching between the density of cross-linking particles and the density of interchain contacts in the solution. The equilibrium between bound- and free nanoparticle would consequently determine whether critical solubility conditions are reached or not. Signi cant effect of light on the degree of binding of particles is thus the key to enlarge the region of light-responsiveness in the phase diagram shown in Fig. 7.4c. The basic principle to designing highly responsive photocomplexes is presented in Section 7.3.
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Figure 7.4. Associative phase separation of complexes between surfactants and azobenzene-modi ed polymers. (a) Cloud points (CP) determined at xed temperature, xed polymer concentration, and varying concentration of sodium dodecyl sulfate polymer structure cf. Fig. 1). (b) Solutions of modi ed poly(sodium acrylate) (cf. Fig. 7.1) and the surfactant C12E4 at 2 g/L in 0.3 M NaCl after centrifugation. Polymer concentrations are quoted in the gure. (c) Schematic phase diagram at xed temperature showing the enlargement of the two-phase region (drop of demixing) upon increasing the association strength, that is, while turning cis isomers into trans ones. Source of (a): Reprinted with permission from Howley et al., 1997. See color insert.
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