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A more detailed description of the synthesis and characterisation of the individual polystyrene based copolymers will be given in a forthcoming publication.
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Some of the films (e.g., 4a, 4f) peeled from freshly evaporated Cu (θ = 57±3°) as well. However, the same polymer films were stable in water when deposited on older Cu substrates that had θ = 85±1°.
PMAA-PMMA-PMAA block copolymers with the hydrophilic:hydrophobic weight ratio (r = 2Mn PMAA block/Mn PMMA block) in the range 0.2-1.4 were kindly provided by A. A. Karanam and L. Klumperman (Eindhoven University of Technology).
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For PMPS the end-capping in the synthesis of the macroinitiator was determined to be greater than 95% by 1H NMR spectroscopy and size-exclusion analysis.6 For the PS-based copolymers polymerization of the styrene was stopped at <90% conversion during the initial syntheses of the PS central blocks (to prevent excessive thermal degradation of the halide chain ends): (a) Lutz, J. F.; Matyjaszewski, K. Macromol. Chem. Phys. 2002, 203, 1385. (b) Matyjaszewski, K.; Davis, K.; Patten, T. E.; Wei, M. L. Tetrahedron 1997, 53, 15321. Consequently, the probability of any PMPS or PS chains completely without initiatior end-caps (leading to homopolymer contamination) can be expected to be less than 1% (5/100 × 5/100).
For PMPS the end-capping in the synthesis of the macroinitiator was determined to be greater than 95% by 1H NMR spectroscopy and size-exclusion analysis.6 For the PS-based copolymers polymerization of the styrene was stopped at <90% conversion during the initial syntheses of the PS central blocks (to prevent excessive thermal degradation of the halide chain ends): (a) Lutz, J. F.; Matyjaszewski, K. Macromol. Chem. Phys. 2002, 203, 1385. (b) Matyjaszewski, K.; Davis, K.; Patten, T. E.; Wei, M. L. Tetrahedron 1997, 53, 15321. Consequently, the probability of any PMPS or PS chains completely without initiatior end-caps (leading to homopolymer contamination) can be expected to be less than 1% (5/100 × 5/100).
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Kinetic analyses of the polymerizations of OEGMA from the PS and PMPS macroinitiators indicated a close correlation of expected chain growth (M n vs conversion) according to that expected for an ABA block copolymer. SEC analysis showed no obvious bimodality However, in most cases due to discrepancies between the hydrodynamic volumes of the POEGMA blocks with the PS calibrants used for SEC calibration, the SEC curves and distribution plots overlapped in the area of interest.
For an overview of the studies of blends of block copolymers, see: Hamley, I. W. The Physics of Block Copolymers; Oxford University Press: Oxford, 1999; pp 366-373.
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