This file Data_Mesoscopic Morphologies in Frustrated ABC Bottlebrush Block Terpolymers was updated on 2025-1-29 by Shuquan Cui Recommended citation for the data: Cui, Shuquan; Murphy, Elizabeth A; Santra, Subrata; Bates, Frank S; Lodge, Timothy P. (2025). Supporting Data for "Mesoscopic Morphologies in Frustrated ABC Bottlebrush Block Terpolymers". Retrieved from the Data Repository for the University of Minnesota (DRUM), https://doi.org/10.13020/s6pf-4e24 ------------------- GENERAL INFORMATION ------------------- Title of Dataset: Supporting Data for Mesoscopic Morphologies in Frustrated ABC Bottlebrush Block Terpolymers Author Information: Principal Investigator Contact Information Name: Prof. Timothy P. Lodge Institution: University of Minnesota Address: Department of Chemistry, 207 Pleasant St SE, Minneapolis, Minnesota 55455 Email: lodge@umn.edu ORCID: 0000-0001-5916-8834 Principal Investigator Contact Information Name: Prof. Frank S. Bates Institution: University of Minnesota Address: Department of Chemical Engineering and Materials Science, 421 Washington Ave SE, Minneapolis, Minnesota 55455 Email: bates001@umn.edu ORCID: 0000-0003-3977-1278 Associate or Co-investigator Contact information Name: Shuquan Cui Institution: University of Minnesota Address: Department of Chemistry, 207 Pleasant St SE, Minneapolis, Minnesota 55455 Email: cui00123@umn.edu ORCID: 0000-0002-8764-0718 Associate or Co-investigator Contact Information Name: Elizabeth A. Murphy Institution: University of California, Santa Barbara Address: Materials Research Laboratory and Department of Chemistry & Biochemistry, University of California, Santa Barbara, CA 93106, USA Email: emurphy@ucsb.edu ORCID: 0000-0003-0846-7943 Associate or Co-investigator Contact information Name: Subrata Santra Institution: University of Minnesota Address: Department of Chemistry, 207 Pleasant St SE, Minneapolis, Minnesota 55455 Email: ssantra@umn.edu ORCID: 0000-0001-6128-7955 Date of data collection (20230529 - 20240503) Geographic location of data collection (where was data collected?): University of Minnesota and University of California, Santa Barbara Information about funding sources that supported the collection of the data: 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 the NSF through the MRSEC (Award Number DMR-2011401) and the NNCI (Award Number ECCS-2025124) programs. 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). This research also used resources from Sector 11-BM CMS beamline of the National Synchrotron Light Source II, a U.S. Department of Energy (DOE) Office of Science User Facility operated for the DOE Office of Science by Brookhaven National Laboratory under Contract no. DE-SC0012704. -------------------------- SHARING/ACCESS INFORMATION -------------------------- 1. Licenses/restrictions placed on the data: CC0 1.0 Universal http://creativecommons.org/publicdomain/zero/1.0/ 2. Links to publications that cite or use the data: Cui S., Murphy E. A., Santra S., Bates F. S., Lodge T. P., Mesoscopic morphologies in frustrated ABC bottlebrush block terpolymers, ACS Nano, 2025, 19, 1211-1221. https://pubs.acs.org/doi/10.1021/acsnano.4c13416 3. Links to other publicly accessible locations of the data: NA 4. Links/relationships to ancillary data sets: NA 5. Was data derived from another source? No. --------------------- DATA & FILE OVERVIEW --------------------- Purpose Statement: This document describes all data associated with Cui et al. "Mesoscopic Morphologies in Frustrated ABC Bottlebrush Block Terpolymers", classifies data based on different Figures in the paper. Several Figures with just schemes are not included. The sample's ID is provided in a pdf file. Files Contained: 1. Data for Figure 1. SEC for bottlebrushes TXT file 2. Data for Figure 2. SAXS for phase portrait TXT file 3. Data for Figure 3. SAXS and TEM for sample 3-6 TXT file for SAXS data and TIF file for TEM image 4. Data for Figure 4. SAXS for domain spacing calculation TXT file 5. Data for Figure 5. SAXS and TEM for sample 3-3 TXT file for SAXS data and TIF file for TEM image 6. Data for Figure 6. SAXS and TEM for sample 7-2 TXT file for SAXS data and TIF file for TEM image 7. Data for Figure 7. SAXS and TEM for sample 4-6 TXT file for SAXS data and TIF file for TEM image 8. Data for Figure 8. SAXS and TEM for sample 9-2 TXT file for SAXS data and TIF file for TEM image 9. Data for Figure 9. SAXS and TEM for RCCUL samples TXT file for SAXS data and TIF file for TEM image 10. Data for Figure S1. NMR for bottlebrushes .csv 11. Data for Figure S2. SEC for bottlebrushes TXT file 12. Data for Figure S3. DSC for bottlebrushes TXT file 13. Data for Figure S4. SAXS and TEM for diblock bottlebrushes TXT file for SAXS data and TIF file for TEM image 14. Data for Figure S5. SAXS and TEM for sample 5-5 TXT file for SAXS data and TIF file for TEM image 15. Data for Figure S6. SAXS and TEM for sample 3-5 TXT file for SAXS data and TIF file for TEM image 16. Data for Figure S7. SAXS and TEM for sample 7-5 TXT file for SAXS data and TIF file for TEM image 17. Data for Figure S9. SAXS and calculated scattering intensity for sample 2-6 Txt file for SAXS and .csv for calculated scattering intensity. 18. Data for Figure S10. Calculated scattering intensity for sample 7-5 .csv 19. Data for Figure S11. TEM image of defects TIF file 20. Data for Figure S12. SAXS data for sample 4-5 TXT file 21. Data for Figure S13. TEM for sample 4-6 TIF file 22. Data for Figure S14. SAXS for sample 10-2 TXT file 23. Data for Figure S15. SAXS for sample 11-2 TXT file 24. Chemical Structures and Synthesis Route Jpg files from Chemdraw Additional related data collected that was not included in the current data package: None. Are there multiple versions of the dataset? N -------------------------- METHODOLOGICAL INFORMATION -------------------------- Description of methods used for collection, generation, and processing of data: Synthesis and Chemical Characterizations AB diblock bottlebrush copolymers PLA-PEP and ABC triblock bottlebrush terpolymers PLA-PEP-PS were prepared by sequential ring-opening metathesis polymerization (ROMP) of norbornene-functionalized macromonomers, PLA (MMA, Mn = 1780 g/mol, Ɖ = 1.13), PEP (MMP, Mn = 1290 g/mol, Ɖ = 1.11), and PS (MMS, Mn = 1240 g/mol, Ɖ = 1.14), catalyzed by Grubbs 3rd catalyst (G3, synthesized from Grubbs 2nd catalyst bought from Sigma-Aldrich) in anhydrous dichloromethane (DCM). The special details of the polymer synthesis and characterizations were reported in our previous publications. A series of child ABC triblock terpolymers along an isopleth with constant fPEP/fPS but different fPLA in the ternary phase portrait were efficiently synthesized by extending a parent PLA-PEP diblock with the PS block. The Mn of macromonomers and the f of each block in bottlebrushes were characterized using proton nuclear magnetic resonance (1H NMR) spectroscopy with CDCl3 as the solvent on a Bruker Avance III HD nanobay AX-400 spectrometer (400 MHz) with a 60-slot SampleXpress autosampler. The Ð of all polymers was measured by size exclusion chromatography (SEC) with a refractive index (RI) detector and tetrahydrofuran (THF) mobile phase (room temperature, 1.0 mL/min). The Mn of each ABC triblock was calculated based on the f of each block and the Mn of its parent diblock, which was measured by SEC using a Wyatt Technology DAWN Heleos II multiangle laser light scattering (MALS) detector with 658 nm wavelength and a Wyatt OPTILAB T-rEX RI detector (THF, 1.0 mL/min, 25 °C). The refractive index increment (dn/dc) for the diblock bottlebrushes was determined by SEC assuming 100% mass recovery. Differential Scanning Calorimetry (DSC) DSC measurements were carried out on a TA Instrument Q1000. Approximately 5 mg of the sample was loaded into hermetically sealed aluminum Tzero DSC pans (DSC Consumables, Austin, MN). Samples were first cooled to –120 °C and then heated to 150 °C to erase any thermal history. Then the sample was cooled to –120 °C again and reheated to 150 °C. The temperature ramp rate was 10 °C/min. Data collected on the second heating were used for the analysis. Small-Angle X-Ray Scattering (SAXS) SAXS data were predominantly collected at the Characterization Facility, University of Minnesota, using a Xenocs Ganesha instrument equipped with a four-position INSTEC heating stage. Additional experiments were conducted at the Materials Research Laboratory (MRL), BioPACIFIC Materials Innovation Platform of the National Science Foundation, University of California, Santa Barbara, using a custom-built SAXS diffractometer, and at the Brookhaven National Laboratory utilizing synchrotron SAXS. Unless noted, bulk samples were annealed under vacuum at 150 °C for 24 h before measurement. During the measurements, each sample was first equilibrated at a target temperature (usually 80 °C) for 10 min. Transmission Electron Microscopy (TEM) TEM images were obtained on an FEI Tecnai Spirit Bio-Twin TEM with an accelerating voltage of 120 kV. Polymer samples were first loaded in a DSC pan and initially annealed at 150 °C under vacuum for 24 h before cooling to 80 °C for additional annealing for 2 h. Then, samples were cryo-sectioned using Leica EM UC6 ultramicrotome with a Diatome diamond knife and then placed on 400-mesh copper grids. Ultrathin sections (~ 70 nm) were stained with freshly prepared RuO4 solutions for 4 minutes, leading to unstained PEP domain (white), slightly stained PLA domain (gray), and strongly stained PS domain (black). People involved with sample collection, processing, analysis and/or submission: Shuquan Cui - collection, processing and analysis of all data Elizabeth A. Murphy - collection of partial SAXS data Subrata Santra - analysis of data Frank S. Bates - analysis of data Timothy P. Lodge - analysis of data --------------------- DATA TREE ------------------- \---Data_ Mesoscopic Morphologies in Frustrated ABC Bottlebrush Block Terpolymers \---Data_ Mesoscopic Morphologies in Frustrated ABC Bottlebrush Block Terpolymers | README.txt | sample_ids.pdf | +---Chemical Structures and Synthesis Route | ROMP.jpg | +---Figure1 | 2-1.txt | 2-2.txt | 2-3.txt | 2-4.txt | 2-5.txt | 2-6.txt | 2-7.txt | +---Figure2 | 1-1.txt | 1-2.txt | 1-3.txt | 1-4.txt | 1-5.txt | 1-6.txt | 10-1.txt | 10-2.txt | 10-3.txt | 11-1.txt | 11-2.txt | 2-1.txt | 2-2.txt | 2-3.txt | 2-4.txt | 2-5.txt | 2-6.txt | 2-7.txt | 3-1.txt | 3-2.txt | 3-3.txt | 3-4.txt | 3-5.txt | 3-6.txt | 4-1.txt | 4-2.txt | 4-3.txt | 4-4.txt | 4-5.txt | 4-6.txt | 4-7.txt | 5-1.txt | 5-2.txt | 5-3.txt | 5-4.txt | 5-5.txt | 6-1.txt | 6-2.txt | 6-3.txt | 6-4.txt | 6-5.txt | 7-1.txt | 7-2.txt | 7-3.txt | 7-4.txt | 7-5.txt | 8-1.txt | 8-2.txt | 8-3.txt | 8-4.txt | 8-5.txt | 8-6.txt | 8-7.txt | 9-1.txt | 9-2.txt | 9-3.txt | +---Figure3 | Sample3-6.txt | TEM.tif | +---Figure4 | 2-1.txt | 2-2.txt | 2-3.txt | 2-4.txt | 2-5.txt | 2-6.txt | 2-7.txt | 4-1.txt | 4-2.txt | 4-3.txt | 4-4.txt | 4-5.txt | 4-6.txt | 4-7.txt | 5-1.txt | 5-2.txt | 5-3.txt | 5-4.txt | 5-5.txt | +---Figure5 | sample3-3.txt | TEM.tif | +---Figure6 | sample7-2.txt | TEM.tif | +---Figure7 | sample4-6.txt | TEM.tif | +---Figure8 | sample9-2.txt | TEM.tif | +---Figure9 | 10-2.txt | 10-3.txt | 11-2.txt | 4-5.txt | 4-6.txt | 5-2.txt | 5-3.txt | 9-2.txt | 9-3.txt | TEM-sample 11-2.tif | +---FigureS1 | 4-1.csv | 4-6.csv | +---FigureS10 | Calculated intensity.csv | +---FigureS11 | TEM1.tif | TEM2.tif | +---FigureS12 | 4-5-solvent casting-thermo annealing.txt | 4-5-thermo annealing.txt | +---FigureS13 | TEM.tif | +---FigureS14 | 10-2-solvent casting-thermo annealing.txt | 10-2-thermo annealing.txt | +---FigureS15 | 11-2.txt | +---FigureS2 | 4-6-after annealing.txt | 4-6-before annealing.txt | +---FigureS3 | 4-1.txt | 4-7.txt | +---FigureS4 | 2-1.txt | 4-1.txt | 7-1.txt | TEM-HEX.tif | TEM-LAM.tif | +---FigureS5 | sample5-5.txt | TEM.tif | +---FigureS6 | 3-5-140C.txt | 3-5-80C.txt | 3-5-cooling80C.txt | TEM.tif | +---FigureS7 | sample7-5-solvent casting.txt | sample7-5-thermo annealing.txt | TEM.tif | \---FigureS9 2-6.txt Calculated intensity.csv