Dynamics of hydrogen-bonded end groups in bulk polymers revealed by solid-state NMR spectroscopy relaxation dispersion experiments

Abstract The dynamic nature of supramolecular networks of telechelic polymers offers new avenues for the design of novel materials with enhanced melt strength and extensibility, increased energy at break, or self-healing properties. However, monitoring the kinetics of the underlying molecular-level...

Full description

Saved in:
Bibliographic Details
Main Authors: Sophia Thiele, Christopher J. G. Plummer, Laura Piveteau, Holger Frauenrath
Format: Article
Language:English
Published: Nature Portfolio 2025-07-01
Series:Communications Chemistry
Online Access:https://doi.org/10.1038/s42004-025-01597-w
Tags: Add Tag
No Tags, Be the first to tag this record!
_version_ 1849344809218605056
author Sophia Thiele
Christopher J. G. Plummer
Laura Piveteau
Holger Frauenrath
author_facet Sophia Thiele
Christopher J. G. Plummer
Laura Piveteau
Holger Frauenrath
author_sort Sophia Thiele
collection DOAJ
description Abstract The dynamic nature of supramolecular networks of telechelic polymers offers new avenues for the design of novel materials with enhanced melt strength and extensibility, increased energy at break, or self-healing properties. However, monitoring the kinetics of the underlying molecular-level scission-reaggregation events remains challenging, particularly in high-molar-mass polymers in the bulk state. Here, we employ solid-state 1H NMR spectroscopy relaxation dispersion experiments to investigate the aggregation-scission dynamics in poly(ε-caprolactone) modified with oligopeptide end groups that form one-dimensional hydrogen-bonded aggregates. We have successfully determined the timescale of end-group dissociation directly and independently of any relaxation of the polymer segments at different temperatures in the bulk semi-crystalline and melt state. This site-specific, non-destructive method is applicable to entangled, high-molar-mass polymers without chemical modifications or modeling, provides critical insight into the dynamics of supramolecular networks in the bulk state, and promises to be a valuable tool for the directed development of next-generation functional materials.
format Article
id doaj-art-9f6cd94231cf43cabc9421f2779e91e6
institution Kabale University
issn 2399-3669
language English
publishDate 2025-07-01
publisher Nature Portfolio
record_format Article
series Communications Chemistry
spelling doaj-art-9f6cd94231cf43cabc9421f2779e91e62025-08-20T03:42:34ZengNature PortfolioCommunications Chemistry2399-36692025-07-018111110.1038/s42004-025-01597-wDynamics of hydrogen-bonded end groups in bulk polymers revealed by solid-state NMR spectroscopy relaxation dispersion experimentsSophia Thiele0Christopher J. G. Plummer1Laura Piveteau2Holger Frauenrath3École Polytechnique Fédérale de Lausanne (EPFL) Institute of MaterialsÉcole Polytechnique Fédérale de Lausanne (EPFL) Institute of MaterialsÉcole Polytechnique Fédérale de Lausanne (EPFL) Nuclear Magnetic Resonance PlatformÉcole Polytechnique Fédérale de Lausanne (EPFL) Institute of MaterialsAbstract The dynamic nature of supramolecular networks of telechelic polymers offers new avenues for the design of novel materials with enhanced melt strength and extensibility, increased energy at break, or self-healing properties. However, monitoring the kinetics of the underlying molecular-level scission-reaggregation events remains challenging, particularly in high-molar-mass polymers in the bulk state. Here, we employ solid-state 1H NMR spectroscopy relaxation dispersion experiments to investigate the aggregation-scission dynamics in poly(ε-caprolactone) modified with oligopeptide end groups that form one-dimensional hydrogen-bonded aggregates. We have successfully determined the timescale of end-group dissociation directly and independently of any relaxation of the polymer segments at different temperatures in the bulk semi-crystalline and melt state. This site-specific, non-destructive method is applicable to entangled, high-molar-mass polymers without chemical modifications or modeling, provides critical insight into the dynamics of supramolecular networks in the bulk state, and promises to be a valuable tool for the directed development of next-generation functional materials.https://doi.org/10.1038/s42004-025-01597-w
spellingShingle Sophia Thiele
Christopher J. G. Plummer
Laura Piveteau
Holger Frauenrath
Dynamics of hydrogen-bonded end groups in bulk polymers revealed by solid-state NMR spectroscopy relaxation dispersion experiments
Communications Chemistry
title Dynamics of hydrogen-bonded end groups in bulk polymers revealed by solid-state NMR spectroscopy relaxation dispersion experiments
title_full Dynamics of hydrogen-bonded end groups in bulk polymers revealed by solid-state NMR spectroscopy relaxation dispersion experiments
title_fullStr Dynamics of hydrogen-bonded end groups in bulk polymers revealed by solid-state NMR spectroscopy relaxation dispersion experiments
title_full_unstemmed Dynamics of hydrogen-bonded end groups in bulk polymers revealed by solid-state NMR spectroscopy relaxation dispersion experiments
title_short Dynamics of hydrogen-bonded end groups in bulk polymers revealed by solid-state NMR spectroscopy relaxation dispersion experiments
title_sort dynamics of hydrogen bonded end groups in bulk polymers revealed by solid state nmr spectroscopy relaxation dispersion experiments
url https://doi.org/10.1038/s42004-025-01597-w
work_keys_str_mv AT sophiathiele dynamicsofhydrogenbondedendgroupsinbulkpolymersrevealedbysolidstatenmrspectroscopyrelaxationdispersionexperiments
AT christopherjgplummer dynamicsofhydrogenbondedendgroupsinbulkpolymersrevealedbysolidstatenmrspectroscopyrelaxationdispersionexperiments
AT laurapiveteau dynamicsofhydrogenbondedendgroupsinbulkpolymersrevealedbysolidstatenmrspectroscopyrelaxationdispersionexperiments
AT holgerfrauenrath dynamicsofhydrogenbondedendgroupsinbulkpolymersrevealedbysolidstatenmrspectroscopyrelaxationdispersionexperiments