Morphology and dynamics of the poly(ϵ‐caprolactone)‐b‐poly(L‐lactide) diblock copolymer and its inclusion compound with α‐cyclodextrin: A solid‐state 13C NMR study
Abstract
A biodegradable diblock copolymer of poly(ϵ‐caprolactone) (PCL) and poly(L‐lactide) (PLLA) was synthesized and characterized. The inclusion compound (IC) of this copolymer with α‐cyclodextrin (α‐CD) was formed and characterized. Wide‐angle X‐ray diffraction showed that in the IC crystals α‐CDs were packed in the channel mode, which isolated and restricted the individual guest copolymer chains to highly extended conformation. Solid‐state 13C NMR techniques were used to investigate the morphology and dynamics of both the bulk and α‐CD‐IC isolated PCL‐b‐PLLA chains. The conformation of the PCL blocks isolated within the α‐CD cavities was similar to the crystalline conformation of PCL blocks in the bulk copolymer. Spin–lattice relaxation time (T1C) measurements revealed a dramatic difference in the mobilities of the semicrystalline bulk copolymer chains and those isolated in the α‐CD‐IC channels. Carbon‐observed proton spin–lattice relaxation in the rotating frame measurements (T1ρH) showed that the bulk copolymer was phase‐separated, while, in the IC, exchange of proton magnetization through spin‐diffusion between the isolated guest polymer chains and the host α‐CD was not complete. The two‐dimensional solid‐state heteronuclear correlation (HetCor) method was also employed to monitor proton communication in these samples. Intrablock exchange of proton magnetization was observed in both the bulk semicrystalline and IC copolymer samples at short mixing times; however, even at the…
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A detailed study of the crystallization kinetics and morphology of both blocks, and their dependence with composition in a wide range, has not been reported.
“Although these systems have been previously evaluated 30 -35 and morphological studies have been previously performed by SAXS, 24,27,28 a detailed study of the crystallization kinetics and morphology of both blocks, and their dependence with composition in a wide range has not been reported, as far as we are aware.”
From Crystallization Kinetics and Morphology of Biodegradable Double Crystalline PLLA- <i>b</i> -PCL Diblock Copolymers (2010) · cites this paper as [34]
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- Authors
- Porbeni, F. E., Shin, I. D., Shuai, X., Wang, X., White, J. L., Jia, X., & Tonelli, A. E.
- Affiliations
- North Carolina State University (US)
- Campbell University (US)
- Case Western Reserve University (US)
- Corresponding author
- Tonelli, Alan E.
- Venue
- Journal of Polymer Science Part B: Polymer Physics
- Publisher
- Wiley
- Published
- 2005-06-24
- Volume
- 43
- Issue
- 15
- Pages
- 2086-2096
- ISSN
- 0887-6266 (ISSN-L)
- 1099-0488
- OpenAlex
- W2044827386
- Cited by
- 30
- References
- 0
- Citations by year
- 2019: 1 · 2018: 3 · 2017: 1 · 2016: 1 · 2015: 3 · 2013: 3 · 2012: 2
- FWCI
- 1.54
- Type
- journal article
- Language
- en
- Open access
- closed
- Locations
- Journal of Polymer Science Part B Polymer Physics (publishedVersion)
- Topics
- Physical Sciences › Materials Science › Biomaterials › biodegradable polymer synthesis and properties
- Physical Sciences › Chemistry › Organic Chemistry › Supramolecular Chemistry and Complexes
- Life Sciences › Pharmacology, Toxicology and Pharmaceutics › Pharmaceutical Science › Drug Solubulity and Delivery Systems
- Keywords
- diblock copolymers, α-cyclodextrin, inclusion compounds, host-guest complexation, polymer morphology, polymer chain dynamics, spin-lattice relaxation, spin diffusion, proton exchange, phase separation, semicrystalline polymers, biodegradable polymers, solid-state 13C NMR
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