Transmission Electron Microscopy Methodology to Analyze Polymer Structure with Submolecular Resolution

Idan Biran; Lothar Houben; Anna Kossoy; Boris Rybtchinski

doi:10.1021/acs.jpcc.3c06977

Transmission Electron Microscopy Methodology to Analyze Polymer Structure with Submolecular Resolution

Idan Biran, Lothar Houben^*, Anna Kossoy, Boris Rybtchinski^*

^*Corresponding author for this work

Research output: Contribution to journal › Article › peer-review

Abstract

The crystallinity of polymeric materials defines their properties, in particular, the mechanical ones. High-resolution transmission electron microscopy (TEM) imaging of polymers would be critical to address intricate polymer crystallinity, yet it is challenging due to polymer sensitivity to the electron beam. We performed high-resolution TEM imaging of polycaprolactone (PCL) thin films employing low-dose focal series reconstruction (LDFSR). LDFSR enabled submolecular resolution imaging of polymer crystals. The direct imaging study was augmented by scanning nanobeam electron diffraction (NBED) using the 4D STEM technique to map micro- and nanoscale crystalline domains. Employing LDFSR combined with 4D STEM, we directly observed interacting polymer chains in the crystal lattice, elucidating the crystal structure with a high degree of precision including lattice deformations. We also imaged PCL lamella using conventional TEM. Our methodology enables long-sought insights into the polymer structure, introducing a new tool for high resolution studies of polymer crystallinity that fills a critical gap in the structural science of polymer materials.

Original language	English
Pages (from-to)	5988-5995
Number of pages	8
Journal	Journal of Physical Chemistry C
Volume	128
Issue number	14
Early online date	28 Mar 2024
DOIs	https://doi.org/10.1021/acs.jpcc.3c06977
Publication status	Published - 11 Apr 2024

Funding

This work was supported by Minerva Foundation and Israel Science Foundation. We also acknowledge Wolfson Family Charitable Trust & The Wolfson Foundation, and Tom and Mary Beck Center for Advanced and Intelligent Materials for financial support. We thank the Tamar Segal-Peretz group (Technion - Israel Institute of Technology) and, in particular, Assaf Simon from this group for helping with TEM sample preparation. L.H. and A.K. are grateful for the support of the Irving and Cherna Moskowitz Center for Nano and Bio-Imaging at the Weizmann Institute of Science. Publisher Copyright: © 2024 The Authors. Published by American Chemical Society.

All Science Journal Classification (ASJC) codes

Electronic, Optical and Magnetic Materials
General Energy
Physical and Theoretical Chemistry
Surfaces, Coatings and Films

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Cite this

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abstract = "The crystallinity of polymeric materials defines their properties, in particular, the mechanical ones. High-resolution transmission electron microscopy (TEM) imaging of polymers would be critical to address intricate polymer crystallinity, yet it is challenging due to polymer sensitivity to the electron beam. We performed high-resolution TEM imaging of polycaprolactone (PCL) thin films employing low-dose focal series reconstruction (LDFSR). LDFSR enabled submolecular resolution imaging of polymer crystals. The direct imaging study was augmented by scanning nanobeam electron diffraction (NBED) using the 4D STEM technique to map micro- and nanoscale crystalline domains. Employing LDFSR combined with 4D STEM, we directly observed interacting polymer chains in the crystal lattice, elucidating the crystal structure with a high degree of precision including lattice deformations. We also imaged PCL lamella using conventional TEM. Our methodology enables long-sought insights into the polymer structure, introducing a new tool for high resolution studies of polymer crystallinity that fills a critical gap in the structural science of polymer materials.",

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N2 - The crystallinity of polymeric materials defines their properties, in particular, the mechanical ones. High-resolution transmission electron microscopy (TEM) imaging of polymers would be critical to address intricate polymer crystallinity, yet it is challenging due to polymer sensitivity to the electron beam. We performed high-resolution TEM imaging of polycaprolactone (PCL) thin films employing low-dose focal series reconstruction (LDFSR). LDFSR enabled submolecular resolution imaging of polymer crystals. The direct imaging study was augmented by scanning nanobeam electron diffraction (NBED) using the 4D STEM technique to map micro- and nanoscale crystalline domains. Employing LDFSR combined with 4D STEM, we directly observed interacting polymer chains in the crystal lattice, elucidating the crystal structure with a high degree of precision including lattice deformations. We also imaged PCL lamella using conventional TEM. Our methodology enables long-sought insights into the polymer structure, introducing a new tool for high resolution studies of polymer crystallinity that fills a critical gap in the structural science of polymer materials.

AB - The crystallinity of polymeric materials defines their properties, in particular, the mechanical ones. High-resolution transmission electron microscopy (TEM) imaging of polymers would be critical to address intricate polymer crystallinity, yet it is challenging due to polymer sensitivity to the electron beam. We performed high-resolution TEM imaging of polycaprolactone (PCL) thin films employing low-dose focal series reconstruction (LDFSR). LDFSR enabled submolecular resolution imaging of polymer crystals. The direct imaging study was augmented by scanning nanobeam electron diffraction (NBED) using the 4D STEM technique to map micro- and nanoscale crystalline domains. Employing LDFSR combined with 4D STEM, we directly observed interacting polymer chains in the crystal lattice, elucidating the crystal structure with a high degree of precision including lattice deformations. We also imaged PCL lamella using conventional TEM. Our methodology enables long-sought insights into the polymer structure, introducing a new tool for high resolution studies of polymer crystallinity that fills a critical gap in the structural science of polymer materials.

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Transmission Electron Microscopy Methodology to Analyze Polymer Structure with Submolecular Resolution

Abstract

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