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Patterson, Joseph P.;Kelley, Elizabeth G.;Murphy, Ryan;Moughton, Adam O.;Robin, Matthew P.; Lu, Annhelen; Colombani, Olivier;Chassenieux,, Chrisophe; Cheung, David L;, Epps, Thomas H.;O'Reilly, Rachel .
Structural Characterization of Amphiphilic Homopolymer Micelles Using Light Scattering, SANS, and Cryo-TEM
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We report the aqueous solution self-assembly of a series of poly(N-isopropylacrylamide) (PNIPAM) polymers end-functionalized with a hydrophobic sulfur–carbon–sulfur (SCS) pincer ligand. Although the hydrophobic ligand accounted for <5 wt % of the overall homopolymer mass, the polymers self-assembled into well-defined spherical micelles in aqueous solution, and these micelles are potential precursors to solution-assembled nanoreactors for small molecule catalysis applications. The micelle structural details were investigated using light scattering, cryogenic transmission electron microscopy (cryo-TEM), and small angle neutron scattering (SANS). Radial density profiles extracted from the cryo-TEM micrographs suggested that the PNIPAM chains formed a diffuse corona with a radially decreasing corona density profile and provided valuable a priori information about the micelle structure for SANS data modeling. SANS analysis indicated a similar profile in which the corona surrounded a small hydrophobic core containing the pincer ligand. The similarity between the SANS and cryo-TEM results demonstrated that detailed information about the micelle density profile can be obtained directly from cryo-TEM and highlighted the complementary use of scattering and cryo-TEM in the structural characterization of solution assemblies, such as the SCS pincer-functionalized homopolymers described here.
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