Confinement and Processing Can Alter the Morphology and Periodicity of Bottlebrush Block Copolymers in Thin Films

Sunday, Daniel F.; Dolejsi, Moshe; Chang, Alice B.; Richter, Lee J.; Li, Ruipeng; Kline, R. Joseph; Nealey, Paul F.; Grubbs, Robert H.

doi:10.1021/acsnano.0c07777

Title: Confinement and Processing Can Alter the Morphology and Periodicity of Bottlebrush Block Copolymers in Thin Films

Journal Article · Mon Nov 23 00:00:00 EST 2020 · ACS Nano

DOI:https://doi.org/10.1021/acsnano.0c07777· OSTI ID:1763323

^[1]; Dolejsi, Moshe ^[2]; Chang, Alice B. ^[3];

^[1]; Li, Ruipeng ^[4]; Kline, R. Joseph ^[1];

^[2];

^[3]

National Inst. of Standards and Technology (NIST), Gaithersburg, MD (United States)
Univ. of Chicago, IL (United States)
California Inst. of Technology (CalTech), Pasadena, CA (United States)
Brookhaven National Lab. (BNL), Upton, NY (United States). National Synchrotron Light Source II (NSLS-II)

Bottlebrush block copolymers (BBCPs) are intriguing architectural variations on linear BCPs with highly tunable structure. Confinement can have a significant impact on polymer assembly, giving rise to changes in morphology, assembly kinetics, and properties like the glass transition. Given that confinement leads to significant changes in the persistence length of bottlebrush homopolymers, it is reasonable to expect that BBCPs will see significant changes in their structure and periodicity relative to the bulk morphology. Understanding how confinement influences assembly will be important for designing BBCPs for thin film applications including membranes, integrated photonic structures, and potentially BCP lithography. In this work, in order to study the effects of confinement on BBCP conformation and morphology, a blade coating was used to prepare films with continuous variation in film thickness. Unlike thin films of linear BCPs, islands/holes were not observed, and instead mixtures of parallel and perpendicular morphologies emerge after annealing. The lamellar periodicity ($$L_0$$) of the morphologies is found to be thickness dependent, increasing $$L_0$$ with decreasing film thickness for blade coated films. Films coated out of tetrahydrofuran (THF) resulted in a single well-defined lamellar periodicity, verified through atomic force microscopy (AFM) and grazing incidence small-angle X-ray scattering (GISAXS), which increases dramatically from the bulk value (30.6 nm) and continues to increase as the film thickness decreases. The largest observed $$L_0$$ was 65.5 nm, and this closely approaches the estimated upper limit of 67 nm corresponding to a fully extended backbone in a bilayer arrangement. Films coated out of propylene glycol methyl ether acetate (PGMEA) resulted in a mixture of perpendicular lamellae and a smaller, likely cylindrical morphology. The lamellar portion of the film shows the same thickness dependence as the lamellae observed in the THF coated films. The scaling of the lamellar $$L_0$$ with respect to film thickness follows predictions for confined semiflexible polymers with weak excluded volume interactions and can be related to models for confinement of DNA. Spin coated films shows the same reduction in periodicity, although at very different film thicknesses. This result suggests that the material has shallow free-energy barriers to transitioning between different $$L_0$$ and morphologies, a property that could be taken advantage of for patterning diverse structures with a single material.

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Research Organization:: Brookhaven National Lab. (BNL), Upton, NY (United States). National Synchrotron Light Source II (NSLS-II); Argonne National Lab. (ANL), Argonne, IL (United States). Advanced Photon Source (APS); Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Advanced Light Source (ALS)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES); E. I. DuPont de Nemours & Co.; The Dow Chemical Company; Northwestern University; National Institute of Standards and Technology (NIST)

Grant/Contract Number:: SC0012704; AC02-06CH11357; AC02-05CH11231; 70NHNB14H012

OSTI ID:: 1763323

Report Number(s):: BNL-220911-2021-JAAM

Journal Information:: ACS Nano, Vol. 14, Issue 12; ISSN 1936-0851

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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36 MATERIALS SCIENCE
bottlebrush
block copolymer
confinement
thin film
self-assembly
saxs
gisaxs

Title: Confinement and Processing Can Alter the Morphology and Periodicity of Bottlebrush Block Copolymers in Thin Films

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