This file Data_Core Shell Gyroid in ABC Bottlebrush Block Terpolymers was updated on 2023-5-22 by Shuquan Cui ------------------- GENERAL INFORMATION ------------------- Title of Dataset: Supporting data for Core−Shell Gyroid in 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 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 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 Associate or Co-investigator Contact Information Name: Bo Zhang Institution: University of Minnesota Address: Department of Chemical Engineering and Materials Science, 421 Washington Ave SE, Minneapolis, Minnesota 55455 Email: zhan5777@umn.edu Associate or Co-investigator Contact Information Name: Liyang Shen Institution: University of Minnesota Address: Department of Chemical Engineering and Materials Science, 421 Washington Ave SE, Minneapolis, Minnesota 55455 Email: shen0481@umn.edu Date of data collection (20210917 - 20220430) Geographic location of data collection (where was data collected?): University of Minnesota 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 NSF through the MRSEC program. Synchrotron SAXS experiments were performed at the 12-ID-B 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. -------------------------- SHARING/ACCESS INFORMATION -------------------------- Suggested Citation for dtaaset: Cui, Shuquan; Zhang, Bo; Shen, Liyang; Bates, Frank S; Lodge, Timothy P. (2023). Supporting data for Core−Shell Gyroid in ABC Bottlebrush Block Terpolymers. Retrieved from the Data Repository for the University of Minnesota, https://doi.org/10.13020/reqb-y062 1. Licenses/restrictions placed on the data: CC0 1.0 Universal 2. Links to publications that cite or use the data: Cui, S. Q.; Zhang, B.; Shen, L. Y.; Bates, F. S.; Lodge, T. P., Core-shell gyroid in ABC bottlebrush block terpolymers, J. Am. Chem. Soc. 2022, 144, 21719-21727. https://doi.org/10.1021/jacs.2c09674 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. "Core−Shell Gyroid in ABC Bottlebrush Block Terpolymers", classifies data based on different Figures in the paper. Several Figures with just schemes are not included. The bottlebrush block polymers are identified by BB(fA/fB, fC), where fA, fB, and fC denote the volume fraction of A, B, and C block, respectively. Files Contained: 1. Data for Figure 1. 1H NMR spectra for three macromonomers Nuclear magnetic resonance (NMR) data from three macromonomers are in Excel workbooks. 2. Data for Figure 2. SEC profiles Txt files with size-exclusion chromatography (SEC) data 3. Data for Figure 3. SAXS_Diblock Small-angle X-ray scattering (SAXS) data. Txt files are recorded by Ganesha SAXS at the University of Minnesota; Dat files are from 12-ID-B beamlines at APS. 4. Data for Figure 4. SAXS data for diblock phase portrait Txt files are recorded by Ganesha SAXS at the University of Minnesota; Dat files are from 12-ID-B beamlines at APS. 5. Data for Figure 5. SAXS data for triblock phase portrait (highlight region) Txt files are recorded by Ganesha SAXS at the University of Minnesota; Dat files are from 12-ID-B beamlines at APS. 6. Data for Figure 6. Typical SAXS data Txt files are recorded by Ganesha SAXS at the University of Minnesota; Dat files are from 12-ID-B beamlines at APS. 7. Data for Figure 7. DSC PEO crystallinity is in an Excel workbook, and caliculated from txt files in the folder "Data for Figure S11. DSC". 8. Data for Figure 8. GYR SAXS Dat files are from 12-ID-B beamlines at APS. 9. Data for Figure S1. 1H NMR_PI-OH Excel workbook 10. Data for Figure S2. 1H NMR_PEP-OH Excel workbook 11. Data for Figure S3. 1H NMR_PS-OH Excel workbook 12. Data for Figure S4. 1H NMR_G3 Excel workbook 13. Data for Figure S5. 1H NMR_Bottlebrush Excel workbook 14. Data for Figure S6. SEC profiles Txt file 15. Data for Figure S7. DSC_Diblock Txt file 16. Data for Figure S8. SEC for thermo-stability Txt file 17. Data for Figure S9. SAXS_Diblock Txt files are recorded by Ganesha SAXS at the University of Minnesota; Dat files are from 12-ID-B beamlines at APS. 18. Data for Figure S10. SAXS_Triblock Txt files are recorded by Ganesha SAXS at the University of Minnesota; Dat files are from 12-ID-B beamlines at APS. 19. Data for Figure S11. DSC Txt file 20. Data for Figure S12. GYR_TEM&SAXS A tiff file collected by FEI Tecnai Spirit Bio-Twin transmission electron microscopy (TEM); a dat file from 12-ID-B beamlines at APS. 21. Data for Figure S13. SAXS_solvent casting Dat file from 12-ID-B beamlines at APS. 22. 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: Details of polymer synthesis were provided in paper "Core−Shell Gyroid in ABC Bottlebrush Block Terpolymers". Chemical structures of all polymers were characterized using proton nuclear magnetic resonance (1H NMR) spectroscopy in CDCl3 unless otherwise noted. Data were collected on a Bruker Avance III HD nanobay AX-400 spectrometer (400 MHz) with a 60-slot SampleXpress autosampler. The molar-mass dispersity 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 number-average molecular weight (Mn) of each triblock was calculated based on the number-average molecular weight (Mn) of its parent diblock, which was measured by SEC with 2 Phenogel columns and a Wyatt Dawn Heleos II multi-angle light scattering (LS) detector as well as a RI detector with THF as the mobile phase (room temperature, 1.0 mL/min). Small-angle X-ray scattering (SAXS) SAXS experiments were conducted either at the Advanced Photon Source (APS) at Argonne National Laboratory, Sector 12-ID-B beamline, or in the Characterization Facility, University of Minnesota, using a Xenocs instrument (Ganesha) equipped with a four-position heating stage (INSTEC). Unless noted, all samples were pre-annealed under vacuum at 150 °C for 48 h before measurement. During SAXS measurements, each sample was first annealed at a target temperature for 5-15 min. The exposure time was 1 s or 5-10 min for measurement at APS or using the Ganesha, respectively. At APS, samples were sealed in differential scanning calorimetry (DSC) pans, while using Ganesha, the samples were sandwiched between two Kapton films, a Viton o-ring, and two Teflon washers, and were sealed in a stainless-steel sandwich cell. Transmission electron microscopy (TEM) TEM images were collected on an FEI Tecnai Spirit Bio-Twin TEM operating at 120 kV. Samples were cryo-sectioned at –70 °C using Leica EM UC6 ultramicrotome with a Diatome diamond knife and placed on 400 mesh copper grids. Ultrathin sections (< 100 nm) were then stained with freshly prepared RuO4 solutions for 5 minutes. PS and PEO domains are preferentially stained. Before microtoming, polymer samples were annealed at 150 °C for 48 h. DSC DSC measurements were conducted on a TA Instruments Q1000. Approximately 5-8 mg of 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 and reheated to 150 °C at a ramp rate of 10 °C/min. The data collected on the second heating was used to determine the glass transition temperature (Tg) and crystallinity. People involved with sample collection, processing, analysis and/or submission: Shuquan Cui - collection, processing and analysis of all data Bo Zhang - collection of partial SAXS data Liyang Shen - collection of all TEM data Frank S. Bates - analysis of data Timothy P. Lodge - analysis of data ----------------------------- Data tree ----------------------------- | README.txt +++Data_Core Shell Gyroid in ABC Bottlebrush Block Terpolymers.rar +---Chemical Structures and Synthesis Route | G3.jpg | Macromonomer PEO.jpg | Macromonomer PEP.jpg | Macromonomer PS.jpg | Ring-opening metathesis polymerization.jpg | +---Data for Figure 1. 1H NMR spectra for three macromonomers | MM_PEO.csv | MM_PEP.csv | MM_PS.csv | +---Data for Figure 2. SEC profiles | Bottlebrush_homo PEP.txt | Bottlebrush_PEP-PS-PEO.txt | Bottlebrush_PEP-PS.txt | MM_PEO.txt | MM_PEP.txt | MM_PS.txt | +---Data for Figure 3. SAXS_Diblock | BB(0.79, 0.00) 140C.dat | BB(1.56, 0.00) 140C.txt | BB(1.56, 0.00) 80C.txt | +---Data for Figure 4. SAXS data for diblock phase portrait | BB(0.25,0.00) 140C.dat | BB(0.32,0.00) 140C.txt | BB(0.33,0.00) 140C.txt | BB(0.33,0.00) 140C_low MW.dat | BB(0.35, 0.00) 80C.txt | BB(0.35,0.00) 140C.txt | BB(0.41, 0.00) 140C.txt | BB(0.41, 0.00) 140C_low MW.dat | BB(0.43, 0.00) 140C.txt | BB(0.43, 0.00) 140C_low MW.txt | BB(0.43, 0.00) 80C.txt | BB(0.43, 0.00) 80C_low MW.txt | BB(0.52,0.00) 140C.dat | BB(0.64,0.00) 140C.dat | BB(0.75,0.00) 140C.txt | BB(0.79,0.00) 140C.dat | BB(0.96,0.00) 140C.dat | BB(1.00,0.00) 140C.dat | BB(1.08,0.00) 140C.dat | BB(1.27,0.00) 140C.dat | BB(1.33,0.00) 140C.txt | BB(1.33,0.00) 80C.txt | BB(1.56, 0.00) 140C_low MW.txt | BB(1.56, 0.00) 80C_low MW.txt | BB(1.56,0.00) 140C.txt | BB(1.86,0.00) 140C.txt | BB(1.86,0.00) 140C_low MW.txt | BB(1.86,0.00) 80C_low MW.txt | BB(2.33,0.00) 140C.txt | BB(2.45,0.00) 140C.txt | +---Data for Figure 5. SAXS data for triblock phase portrait (highlight region) | BB(1.00, 0.00) 140C.dat | BB(1.00, 0.13) 140C.dat | BB(1.00, 0.16) 140C.dat | BB(1.00, 0.19) 140C.dat | BB(1.00, 0.23) 140C.dat | BB(1.08, 0.00) 140C.dat | BB(1.08, 0.04) 140C.dat | BB(1.08, 0.08) 140C.dat | BB(1.27, 0.00) 140C.dat | BB(1.27, 0.07) 140C.dat | BB(1.27, 0.10) 140C..dat | BB(1.27, 0.14) 140C..dat | BB(1.27, 0.15) 140C..dat | BB(1.27, 0.17) 140C..dat | BB(1.27, 0.21) 140C..dat | BB(1.27, 0.23) 140C..dat | BB(1.27, 0.24) 140C..dat | BB(1.27, 0.27) 140C..dat | BB(1.56, 0.00) 140C.txt | BB(1.56, 0.06) 140C.txt | BB(1.56, 0.10) 140C.txt | BB(1.56, 0.13) 140C.txt | BB(1.56, 0.14) 140C.txt | BB(1.56, 0.19) 140C.txt | BB(1.56, 0.23) 140C.txt | BB(1.56, 0.24) 140C.txt | BB(1.56, 0.28) 140C.txt | BB(1.86, 0.00) 140C.txt | BB(1.86, 0.06) 140C.txt | BB(1.86, 0.10) 140C.txt | BB(1.86, 0.12) 140C.txt | BB(1.86, 0.15) 140C.txt | BB(1.86, 0.19) 140C.txt | BB(1.86, 0.23) 140C.txt | BB(1.86, 0.24) 140C.txt | BB(1.86, 0.28) 140C.txt | +---Data for Figure 6. Typical SAXS data | BB(1.00, 0.23) 140C.dat | BB(1.08, 0.04) 140C.dat | BB(1.56, 0.00) 140C.txt | BB(1.86, 0.15) 140C.txt | +---Data for Figure 7. DSC | PEO crystallinity.xlsx | +---Data for Figure 8. GYR SAXS | BB(1.27, 0.10) 140C..dat | BB(1.27, 0.14) 140C..dat | BB(1.27, 0.15) 140C..dat | BB(1.27, 0.17) 140C..dat | BB(1.27, 0.21) 140C..dat | BB(1.27, 0.23) 140C..dat | BB(1.27, 0.24) 140C..dat | BB(1.27, 0.27) 140C..dat | +---Data for Figure S1. 1H NMR_PI-OH | PI-OH.csv | +---Data for Figure S10. SAXS_Triblock | BB(1.00, 0.00) 140C.dat | BB(1.00, 0.13) 140C.dat | BB(1.00, 0.16) 140C.dat | BB(1.00, 0.19) 140C.dat | BB(1.00, 0.23) 140C.dat | BB(1.56, 0.00) 140C.txt | BB(1.56, 0.06) 140C.txt | BB(1.56, 0.10) 140C.txt | BB(1.56, 0.13) 140C.txt | BB(1.56, 0.14) 140C.txt | BB(1.56, 0.19) 140C.txt | BB(1.56, 0.23) 140C.txt | BB(1.56, 0.24) 140C.txt | BB(1.56, 0.28) 140C.txt | BB(1.86, 0.00) 140C.txt | BB(1.86, 0.06) 140C.txt | BB(1.86, 0.10) 140C.txt | BB(1.86, 0.12) 140C.txt | BB(1.86, 0.15) 140C.txt | BB(1.86, 0.19) 140C.txt | BB(1.86, 0.23) 140C.txt | BB(1.86, 0.24) 140C.txt | BB(1.86, 0.28) 140C.txt | +---Data for Figure S11. DSC | BB(1.56, 0.00).txt | BB(1.56, 0.06).txt | BB(1.56, 0.10).txt | BB(1.56, 0.13).txt | BB(1.56, 0.14).txt | BB(1.56, 0.19).txt | BB(1.56, 0.23).txt | BB(1.56, 0.24).txt | BB(1.56, 0.28).txt | +---Data for Figure S12. GYR_TEM&SAXS | BB(1.00, 0.19) 140C.dat | TEM_GYR.tif | +---Data for Figure S13. SAXS_solvent casting | BB(1.00, 0.19) 140C_solvent casting.dat | BB(1.00, 0.19) 140C_thermo-annealing.dat | +---Data for Figure S2. 1H NMR_PEP-OH | PEP-OH.csv | +---Data for Figure S3. 1H NMR_PS-OH | PS-OH.csv | +---Data for Figure S4. 1H NMR_G3 | G3.csv | +---Data for Figure S5. 1H NMR_Bottlebrush | Homo PEP.csv | PEP-PS-PEO.csv | PEP-PS.csv | +---Data for Figure S6. SEC profiles | BB(1.00, 0.00).txt | +---Data for Figure S7. DSC_Diblock | BB(1.00, 0.00).txt | +---Data for Figure S8. SEC for thermo-stability | BB(0.79,0.19)_after annealing.txt | BB(0.79,0.19)_as synthesized.txt | BB(1.08,0.00)_after annealing.txt | BB(1.08,0.00)_as synthesized.txt | \---Data for Figure S9. SAXS_Diblock BB(0.35, 0.00) 80C.txt BB(0.35,0.00) 140C.txt BB(0.52,0.00) 140C.dat BB(1.08,0.00) 140C.dat BB(1.56,0.00) 140C.txt BB(1.86,0.00) 80C_low MW.txt