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Cited by 87Block Copolymer Self-AssemblyPolymer crystallization and propertiesAdvanced Polymer Synthesis and Characterization

Synthesis and Characterization of Polystyrene- b -poly(ethylene oxide)- b -poly(ε-caprolactone) Block Copolymers

Arnal, M. L., Balsamo, V., López-Carrasquero, F., Contreras, J., Carrillo, M., Schmalz, H., Abetz, V., Laredo, E. +1 more·2001·Macromolecules
DOI 10.1021/ma011058g
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Abstract

The preparation of polystyrene- b -poly(ethylene oxide)- b -poly(ε-caprolactone) triblock copolymers using three different strategies is described. Experimentally, a method we have called “thermal” is the simplest one of the three employed. However, it presents serious limitations for the preparation of high molecular weight triblock copolymers with low polydispersity. The titration method is a more elegant alternative to prepare the PS- b -PEO- b -PCL triblock copolymers. Nevertheless, the stoichiometric titration of the precursor terminal hydroxyl groups requires much expertise, and it becomes more difficult as the concentration of such terminal groups decreases when the precursor molecular weight increases. Finally, the sequential method may be regarded as the most convenient one. However, the experimental steps involved a solvent exchange during polymerization that must be performed under conditions of strict purity and high vacuum. Several triblock and pentablock copolymers of varying compositions and molecular weights were successfully prepared. The fact that these copolymers contain two crystallizable blocks, i.e., PEO and PCL, makes them very interesting from a structural point of view. The copolymers were found to be phase segregated according to evidence provided by DSC and WAXS. The crystallization and melting behavior of both PEO and PCL blocks is greatly affected by composition. Fractionated crystallization phenomena were detected when either one or both blocks constituted the minor components within the block copolymers.

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  • In strongly segregated systems (high χN values, T_ODT > Tg > Tc), the phase segregated structure of the melt is preserved, but the amorphous block is in the glassy state, so crystallization of the crystalline block occurs under hard confinement.

    “The phase segregated structure of the melt is preserved, but in this case, the amorphous block is in the glassy state, therefore the crystallization process of the crystalline block occurs under hard confinement (the same behaviour is observed for double crystalline diblock copolymers, once the first block crystallizes, the second one crystallizes under hard confinement) [ 101 , 104 , 105 , 108 ,”

    From Fractionated crystallization in semicrystalline polymers (2021) · cites this paper as [132]

  • The PCL block within L81C19 crystallizes by homogeneous nucleation, with crystal growth essentially instantaneous so that the kinetics is entirely controlled by the nucleation process.

    “This result confirms that the PCL block crystallizes by homogeneous nucleation, that is, that crystal growth must be essentially instantaneous so the kinetics is entirely controlled by the nucleation process. 17,79”

    From Crystallization Kinetics and Morphology of Biodegradable Double Crystalline PLLA- <i>b</i> -PCL Diblock Copolymers (2010) · cites this paper as [79]

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Authors
Arnal, M. L., Balsamo, V., López-Carrasquero, F., Contreras, J., Carrillo, M., Schmalz, H., Abetz, V., Laredo, E., & Müller, A. J.
Affiliations
  • Universidad de Los Andes (VE)
  • Grupo de Polímeros USB, Departamento de Ciencia de los Materiales, Universidad Simón Bolívar, Apartado 89000, Caracas 1080A, Venezuela; Grupo de Polímeros ULA, Departamento de Química, Facultad de Ciencias, Universidad de los Andes, Mérida 5101A, Venezuela; Makromolekulare Chemie II, Universität Bayreuth, 95440 Bayreuth, Germany; and Grupo de Física de Sólidos USB, Departamento de Física, Universidad Simón Bolívar, Apartado 89000, Caracas 1080A, Venezuela
ORCID
Venue
Macromolecules
Publisher
American Chemical Society (ACS)
Published
2001-10-04
Volume
34
Issue
23
Pages
7973-7982
ISSN
  • 0024-9297 (ISSN-L)
  • 1520-5835
DOI
10.1021/ma011058g
OpenAlex
W2042472102
Cited by
87
References
31
Citations by year
2026: 1 · 2021: 2 · 2020: 3 · 2019: 1 · 2018: 1 · 2017: 5 · 2016: 3 · 2015: 5 · 2014: 8 · 2013: 5 · 2012: 5
FWCI
4.58
Type
journal article
Language
en
Open access
closed
Locations
Macromolecules (publishedVersion)
Topics
  • Physical Sciences › Materials Science › Materials Chemistry › Block Copolymer Self-Assembly
  • Physical Sciences › Materials Science › Polymers and Plastics › Polymer crystallization and properties
  • Physical Sciences › Chemistry › Organic Chemistry › Advanced Polymer Synthesis and Characterization
Keywords
triblock copolymers, block copolymer synthesis, titration method, sequential polymerization, thermal polymerization, polydispersity, pentablock copolymers, phase segregation, crystallization behavior, fractional crystallization, molecular weight

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