Supporting Data for Cylinders-in-Undulating-Lamellae Morphology from ABC Bottlebrush Block Terpolymers

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2022-11-29
2023-08-24

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2024-12-31

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Supporting Data for Cylinders-in-Undulating-Lamellae Morphology from ABC Bottlebrush Block Terpolymers

Published Date

2025-01-06

Author Contact

Lodge, Timothy P
lodge@umn.edu

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Dataset
Experimental Data

Abstract

Block polymer self-assembly affords a versatile bottom-up strategy to develop materials with desired properties dictated by specific symmetries and dimensions. Owing to distinct properties compared with linear counterparts, bottlebrush block polymers with side chains densely grafted on a backbone have attracted extensive attention. However, the morphologies found in bottlebrush block polymers so far are limited, and only lamellar and cylindrical ordered phases have been reported in diblock bottlebrushes. The absence of complex morphologies such as networks might originate from the intrinsically stiff backbone architecture. We experimentally investigated the morphologies of non-frustrated ABC bottlebrush block terpolymers, based on two chemistries, poly(ethylene-alt-propylene)-b-polystyrene-b-poly(DL-lactic acid) (PEP-PS-PLA) and PEP-b-PS-b-poly(ethylene oxide) (PEP-PS-PEO) synthesized by ring-opening metathesis polymerization of norbornene-terminated macromonomers. Structural characterization based on small-angle X-ray scattering and transmission electron microscopy measurements revealed an unprecedented cylinders-in-undulating-lamellae (CUL) morphology with p2 symmetry, for both systems. Additionally, automated liquid chromatography was employed to fractionate the PEP-PS-PLA bottlebrush polymer, leading to fractions with a spectrum of morphologies, including the CUL. These findings underscore the significance of macromolecular dispersity in nominally narrow dispersity bottlebrush polymers, while demonstrating the power of this fractionation technique.

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The data folder contains all data of the figures in the article and SI appendix, including nuclear magnetic resonance (NMR), size exclusion chromatography (SEC), differential scanning calorimetry (DSC), small-angle X-ray scattering (SAXS), transmission electron microscopy (TEM), 3D TEM reconstruction, polymer fractionation data. See the readme.txt file for further details.

Referenced by

Cui S. Q., Murphy E. A., Zhang W., Zografos A., Shen L. Y., Bates F. S., Lodge T. P., Cylinders-in-undulating-lamellae morphology from ABC bottlebrush block terpolymers, Journal of the American Chemical Society 2024 (146): 6796-6805.

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This work was supported by the National Science Foundation (NSF) through the University of Minnesota MRSEC under Award DMR-2011401. Parts of this work were carried out in the Characterization Facility, University of Minnesota, which receives partial support from NSF through the MRSEC program. The research reported here was partially supported by the BioPACIFIC Materials Innovation Platform of the National Science Foundation under Award No. DMR-1933487 (equipment and characterization). Synchrotron SAXS experiments were performed at the 5-ID-D beamlines of the Advanced Photon Source (APS). This research used resources of the Advanced Photon Source, a U.S. Department of Energy (DOE) Office of Science User Facility operated for the DOE Office of Science by Argonne National Laboratory under contract no. DE-AC02-06CH11357.

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Cui, Shuquan; Murphy, Elizabeth A; Zhang, Wei; Zografos, Aristotelis; Shen, Liyang; Bates, Frank S; Lodge, Timothy P. (2025). Supporting Data for Cylinders-in-Undulating-Lamellae Morphology from ABC Bottlebrush Block Terpolymers. Retrieved from the Data Repository for the University of Minnesota (DRUM), https://doi.org/10.13020/134v-8d32.

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