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A DSC and XPS characterization of core–shell morphology of block copolymer nanoparticles

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Abstract

Self-assembly of amphiphilic block copolymer chains is known to produce core–shell nanoparticles, but imaging techniques have generally failed to provide clear evidence about the multiphase structure. We report herein the advantages and limitations of modulated temperature differential scanning calorimetry (MDSC) and X-ray photoelectron spectroscopy (XPS) for the morphology study of spherical poly(hydroxyethyl acrylate)-b-polystyrene diblock copolymer nanoparticles with an intensity-average diameter of 40 nm. Using lyophilized particles, MDSC is more informative than XPS since it allows the three morphological features of composite latex particles to be distinguished: polystyrene core, poly(hydroxyethyl acrylate) shell, and interface. In MDSC, phase separation is evidenced by two distinct increments of heat capacity (ΔCp) in the glass transition regions of the two blocks. By measuring ΔCp values, an interface weight fraction of 70% is measured that gradually decreases to 50% with annealing time (150 °C, 2 h), indicating a higher extent of phase separation.

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Acknowledgments

Marc Schmutz and the electron microscopy platform at the Institut Charles Sadron (CNRS, UPR 22, University of Strasbourg) are acknowledged for the cryo-TEM images and the use of the instruments.

Funding

The authors acknowledge the Ministry of Higher Education and Research in France (“Ministère de l’Enseignement Supérieur et de la Recherche” [MESR]) for the PhD fellowship of Vitalii Tkachenko.

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Authors and Affiliations

  1. CNRS, IS2M UMR7361, Université de Haute-Alsace, F-68100, Mulhouse, France

    Vitalii Tkachenko, Ludovic Josien, Gautier Schrodj, Samar Hajjar-Garreau, Julien Poly & Abraham Chemtob

  2. Université de Strasbourg, Strasbourg, France

    Vitalii Tkachenko, Ludovic Josien, Gautier Schrodj, Samar Hajjar-Garreau, Julien Poly & Abraham Chemtob

  3. CNRS, LAGEPP UMR5007, Université Claude Bernard Lyon 1, F-69622, Villeurbanne, France

    Sébastien Urbaniak

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  1. Vitalii Tkachenko
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Correspondence to Julien Poly or Abraham Chemtob.

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Tkachenko, V., Josien, L., Schrodj, G. et al. A DSC and XPS characterization of core–shell morphology of block copolymer nanoparticles. Colloid Polym Sci 298, 1095–1105 (2020). https://doi.org/10.1007/s00396-020-04676-7

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