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We report the synthesis and characterization of well-defined polystyrene-block-poly(vinyl alcohol) (PS-b-PVA) polymers and the corresponding polystyrene-block-poly(vinyl acetate) (PS-b-PVAc) precursors using a combination of atom transfer radical polymerization (ATRP), copper-catalyzed azide alkyne cycloaddition reaction, and reversible addition-fragmentation chain transfer (RAFT) polymerization. Bromine end-functional polystyrene was first prepared using activators regenerated by electron transfer ATRP. A xanthate mediated macro chain transfer agent carrying a triazole-based R-group was achieved by the CuAAC reaction between the corresponding azide-functional polystyrene and an alkyne functional O-ethyl S-prop-2-ynyl carbonodithioate. PS-b-PVAc diblock polymers were synthesized by RAFT polymerization using the triazole-based macro-CTA. The formation of well-defined PS-b-PVA diblock polymers was followed by 1H nuclear magnetic resonance spectroscopy, infrared spectroscopy and size-exclusion chromatography. Thermal properties of the diblock polymer were analyzed by thermal gravimetric analysis and differential scanning calorimetry. The PVAc segments were hydrolyzed to give the corresponding PS-b-PVA block polymers. The morphology of the polymers was investigated by grazing-incidence small-angle scattering as well as atomic force microscopy.
Bibliographical noteFunding Information:
We thank the BASF Corporation for their financial support of this project. SAXS and GISAXS data were obtained at the Advanced Photon Source, a U.S. Department of Energy (DOE) Office of Science User Facility operated for the DOE Office of Science by Argonne National Laboratory. Parts of this work were carried out in the Characterization Facility, University of Minnesota, which receives partial support from National Science Foundation (NSF) through the Materials Research Science and Engineering Centers (MRSEC) program.
© The Royal Society of Chemistry 2018.
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