This README file was updated on 2026-1-5 by Daun Jeong Recommended citation for the data: Jeong, Daun; Cui, Shuquan; Jahan, Nusrat; Ellison, Christopher J.; Bates, Frank S. (2025). Supporting Data for Compatibilization of iPP/PS Blends with Diblock and Triblock Copolymers. Retrieved from the Data Repository for the University of Minnesota (DRUM), https://doi.org/10.1021/acs.macromol.5c01877 ------------------- GENERAL INFORMATION ------------------- Title of Dataset: Supporting Data for Compatibilization of iPP/PS Blends with Diblock and Triblock Copolymers Author Information: 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 Principal Investigator Contact Information Name: Prof. Christopher J. Ellison Institution: University of Minnesota Address: Department of Chemical Engineering and Materials Science, 421 Washington Ave SE, Minneapolis, Minnesota 55455 Email: cellison@umn.edu ORCID: 0000-0002-0393-2941 Associate or Co-investigator Contact Information Name: Daun Jeong Institution: University of Minnesota Address: Department of Chemical Engineering and Materials Science, 421 Washington Ave SE, Minneapolis, Minnesota 55455 Email: djeong@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 ORCID: 0000-0002-8764-0718 Associate or Co-investigator Contact Information Name: Nusrat Jahan Institution: University of Minnesota Address: Department of Chemical Engineering and Materials Science, 421 Washington Ave SE, Minneapolis, Minnesota 55455 Email: jahan064@umn.edu Date of data collection: 20240601 - 20241223 Geographic location of data collection: University of Minnesota Information about funding sources that supported the collection of the data: This work was supported by the National Science Foundation under grant DMR-2304179. 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. Parts of this work were carried out in the Polymer Characterization and Processing Facility, University of Minnesota, which has received capital equipment funding from the National Science Foundation through the UMN MRSEC under Award Number DMR-2011401. 1H NMR spectra were collected on a Bruker Avance II HD 400 MHz spectrometer purchased by the Office of the Vice President of Research, the College of Science of and Engineering, and the Department of Chemistry at the University of Minnesota. -------------------------- 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: https://doi.org/10.1021/acs.macromol.5c01877 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 Jeong et al. "Compatibilization of iPP/PS Blends with Diblock and Triblock Copolymers", classifies data based on different Figures in the paper. Figures with just schemes are not included. The sample's ID is provided in a PDF file. Files Contained: 1. Data for Figure 2. TEM data for iPP:PS=80:20 neat blends and iPP:PS=80:20 blends compatibilized with S46X56, S11X62S10, and S52X56S47 block copolymers (1 and 5 wt%) TIF file 2. Data for Figure 3. Stress-strain data for iPP, PS, iPP:PS=80:20 neat blends, and iPP:PS=80:20 blends compatibilized with SX and SXS block copolymers (1, 3, and 5 wt%) Excel workbook 3. Data for Figure 4. Stress-strain data for iPP, PS, iPP:PS=80:20 neat blends, and iPP:PS=80:20 blends compatibilized with SX and SXS block copolymers Excel workbook 4. Data for Figure 5. SEM data for iPP:PS=80:20 neat blends and iPP:PS=80:20 blends compatibilized with S46X56, S11X62S10, and S52X56S47 block copolymers (1 and 5 wt%) TIF file 5. Data for Figure 6. 90o peel test data for iPP/PS laminate without block copolymer and iPP/block copolymer/PS laminates with S46X56, S11X62S10, S52X56S47, and S91X63S76. Excel workbook 6. Data for Figure S1. SEC for the first block, the diblock, and the triblock of the SXS precursor Excel workbook 7. Data for Figure S2. NMR for the diblock and triblock of the SXS precursor Excel workbook 8. Data for Figure S3. SEC for the SXS precursor and the SXS copolymer Excel workbook 9. Data for Figure S4. NMR for the SXS precursor and the SXS copolymer TXT file 10. Data for Figure S5. DSC for the SX and SXS block copolymers Excel workbook 11. Data for Figure S6. Rheology data for the SX and SXS block copolymers Excel workbook 12. Data for Figure S7. TEM data for iPP:PS=80:20 blends compatibilized with S46X56, S11X62S10, and S23X65S21 (1, 3, and 5 wt%) TIF file 13. Data for Figure S8. TEM data for iPP:PS=80:20 blends compatibilized with S33X63S31, S52X56S47, and S91X63S76 (1, 3, and 5 wt%) TIF file 14. Data for Figure S9. Image J statistics data for iPP:PS=80:20 blends compatibilized with S46X56, S11X62S10, and S23X65S21 (1, 3, and 5 wt%) Excel workbook 15. Data for Figure S10. Image J statistics data for iPP:PS=80:20 blends compatibilized with S33X63S31, S52X56S47, and S91X63S76 (1, 3, and 5 wt%) Excel workbook 16. Data for Figure S11. Image J statistics data for iPP:PS=80:20 neat blends and iPP:PS=80:20 blends compatibilized with SX and SXS block copolymers Excel workbook 17. Data for Figures S12. Stress-strain data for iPP, PS, iPP:PS=80:20 neat blends, and compatibilized iPP:PS=80:20 blends with SX diblock (0.1, 0.3, 0.5, and 1 wt%) Excel workbook 18. Data for Figures S13. SEM data for iPP:PS=80:20 + S46X56 compatibilized blends (0.1, 0.3, and 0.5 wt%) TIF file 19. Data for Figure S14. TEM data for iPP:PS=80:20 + 5 wt% S52X56S47 blend after tensile testing TIF file 20. Data for Figure S15. SEM data for iPP:PS=80:20 + 3wt% S46X56, S11X62S10, and S52X56S47 blends TIF file 21. Data for Figure S16. SEM data for delaminated iPP, PS, S46X56, S11X62S10, and S52X56S47 layers TIF file 22. Data for Figure S17. DSC data for iPP, iPP:PS=80:20 neat blends, and iPP:PS=80:20 blends compatiblized with S46X56, S11X62S10, and S52X56S47 Excel workbook 23. Data for Figure S18. Yield strength data for iPP, iPP:PS=80:20 neat blends, and iPP:PS=80:20 blends compatibilized with SX and SXS block copolymers Excel workbook 24. Synthetic Scheme for SXS block copolymers JPG file 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: Materials Commercial homopolymers iPP (PPH 3060, Mn = 162 kg/mol, Đ = 2.2, MFI = 1.8 g/10 min at 230 °C with 2.16 kg) and PS (STYRON 685D, Mn = 127 kg/mol, Đ = 1.96, MFI = 1.5 g/10 min at 200 °C with 5 kg) were supplied by TotalEnergies and Dow Chemical Company, respectively, and used as received. The Mn and Đ of iPP were characterized using an Agilent PL-GPC 220 high-temperature SEC system equipped with a differential refractive index (RI) detector and Wyatt DAWN HELEOS II multiangle light scattering (MALS) detector at a concentration of 1 mg/mL with 1,2,4-trichlorobenzene mobile phase and flow rate of 1 mL/min at 135 °C. The refractive index increment (dn/dc) for iPP was determined by SEC assuming 100% mass recovery. The Mn and Đ of PS were determined using an Agilent Infinity 1260 series HPLC system equipped with a Wyatt differential refractive index detector and 3 Styragel HR columns calibrated with polystyrene standards. The sample concentration was 1 mg/mL with tetrahydrofuran (THF) as the mobile phase and flow rate of 1 mL/min at 35 °C. Cyclohexane (HPLC, Fisher Scientific) and THF (HPLC, Fisher Scientific) used for anionic polymerization were purified by passing through activated alumina columns, with THF further distilled from butylmagnesium chloride solution (2.0 M in THF, Sigma-Aldrich). Benzene (anhydrous, ≥ 99.8%, Sigma-Aldrich) used for anionic polymerization of high molecular weight triblocks was purified over molecular sieves (4 Å, Sigma-Aldrich) and further distilled from n-butyllithium (2.5 M in hexane, Sigma-Aldrich). Styrene (≥99%, Sigma-Aldrich) was purified over CaH2 (≥99.9%, Sigma-Aldrich) overnight and further distilled from n-butylethylmagnesium (0.9 M in heptane, Fisher Scientific) twice. Butadiene (≥99%, Sigma-Aldrich) was twice distilled from n-butyllithium (2.5 M in hexanes, Sigma-Aldrich). Synthesis of Styrene/Butadiene Derived Block Copolymers A series of poly(styrene)-b-poly(ethylene-r-ethylethylene)-b-poly(styrene) (SXS) triblock copolymers with varying S block molecular weight were synthesized by sequential anionic polymerization. Purified cyclohexane or benzene and THF ([THF]:[Li] = 400:1) were first added to the reactor under an argon atmosphere, followed by n-butyllithium initiator and purified styrene monomer, which was allowed to react for 4 h at 20 °C. An aliquot of the living polymer was taken to determine the molecular weight and dispersity. The reactor was cooled to 8 °C and purified butadiene monomer was added, which was allowed to react for an additional 4 to 8 h. After the second reaction, an aliquot of the diblock was also taken from the reactor for analysis, and purified styrene monomer was added. After another 16 h reaction at 20 °C, the living polymer was terminated by degassed methanol and precipitated in methanol three times and dried under vacuum at 30 °C. Termination of the living PS-block-1,2-PB chains with purified methanol led to a diblock copolymer. The synthesized polymers were dissolved in benzene, freeze-dried overnight, and dissolved in purified cyclohexane at a concentration of 3 g/L. Catalytic hydrogenation of the 1,2-PB block was conducted using a homogeneous Ni/Al catalyst (Nickel(II) 2-ethylhexanoate/triethyl aluminum, Sigma-Aldrich) in a high-pressure reactor operated at 100 °C with 500 psi of H2 for 24 h. Catalyst was removed by vigorous stirring with 8% (w/w) citric acid aqueous solution overnight followed by extraction of cyclohexane layer using separatory funnel. The product was precipitated in methanol three times and dried under vacuum at 50 °C to constant weight. Molecular Characterization Mn and Đ of each block of the prepared block copolymers were determined using 1H NMR spectroscopy (Bruker Avance III HD nanobay AX-400 spectrometer, 400 MHz) and SEC (Agilent Infinity 1260 series HPLC system). Mn and Đ of the first polystyrene (PS) block was determined using SEC equipped with an RI detector calibrated with polystyrene standards at a concentration of 1 mg/mL. Comparing the integration values of the 1H NMR spectra peaks corresponding to the PS block and 1,2-PB second block of the diblock aliquot and triblock copolymers, Mns of the second and third blocks were characterized. The 1,2-content of the PB block was determined by 1H NMR spectra (Figure S2). All 1H NMR analyses were conducted with 10 mg/mL CDCl3 solution at room temperature. Thermal Anaylsis Glass transition temperature (Tg), melting temperature (Tm), and crystallinity (Xc) were determined using a TA Instruments Discovery 2500 DSC. Seven to 10 mg of samples were sealed in an aluminum Tzero DSC pans (DSC Consumables, Austin, MN) and tested under a nitrogen atmosphere at a temperature ramp rate of 10 °C/min. Blend Preparation and Tensile Test All Polymer blends were prepared using a recirculating 15 mL DSM Xplore twin-screw microcompounder at 190 °C under a nitrogen purge, operated for 10 min at 130 rpm. The blended materials were molded into 0.5 mm thick films at 180 °C with 5 min annealing followed by pressing at 2000 lb for 5 min using a Wabash hot press. The prepared films were fast cooled (≈ 100 °C/min) by transferring to a second press held at 20 °C. Dumbbell-shaped tensile bars were prepared using a die cutter (ASTM D1708, 5 mm gauge width, 22 mm gauge length) and tested using an Instron 5966 Universal Testing System equipped with a 500 N cell, with a crosshead speed of 22 mm/min (100%/min strain rate) at room temperature. Rheology Bulk rheological properties of the SX and SXS block copolymers were examined using an ARES-G2 rheometer (Thermal Analysis Instruments, New Castle, DE) under a nitrogen gas purge. An 8 mm parallel plate geometry with a 1 mm gap was employed. Frequency sweeps were performed over a range of 0.1 to 100 rad/s at a constant strain amplitude of 1%. Measurements were conducted from 240 to 140 °C in 20 °C decrements, with 10 min intervals between measurements for temperature equilibration. Master curves were generated using time–temperature superposition referenced at 180 °C. Morphological Characterization Phase morphology of neat and compatibilized blends was characterized using an FEI Tecnai Spirit Bio-Twin transmission electron microscopy (TEM) with an accelerating voltage of 120 kV. Thin slices (≈70 nm) of blends were obtained using a Leica EM UC6 ultramicrotome equipped with a Diatome diamond knife at –120 °C. Slices were mounted on a 400-mesh copper grids and stained with Ruthenium tetroxide (RuO4) solution for 5 min, preferentially staining the PS domains. Fracture surfaces of the tensile specimens were examined using a Hitachi SU8230 field emission scanning electron microscope (SEM) operated with an accelerating voltage of 10 kV at approximately 8 mm working distance. Specimens were affixed with carbon tape to a 90° pin stub mount with the fractured surface facing upward and sputter coated with a 5 nm-thick platinum conducting layer to minimize charging effects. 90° Peel Testing Laminated PS/block copolymer/iPP samples were prepared through a three-step fabrication procedure. All polymers were annealed for 5 min at 180 °C without pressure using a Wabash hot press. Polymer pellets of iPP (PPH 3060) and PS (STYRON 685D) were pressed into 1 cm × 13 cm × 0.5 mm and 10 cm × 10 cm × 2 mm films using a stainless steel mold, between Teflon sheets using a Wabash hot press at 180 °C with 2000 lb for 5 min, and quenched by transferring to a water-cooled second press. Block copolymer powders were pressed using a Wabash hot press between Teflon sheets at 180 °C under 10 tons of force for 5 min and quenched in the same manner. The film thickness was measured by calipers to be between 30 to 60 μm and trimmed to 5 cm × 5 cm. All film surfaces were wiped with a Kim-wipe soaked in methanol before lamination. The molded block copolymer film was placed over the middle and top half of the PS plate (10 cm × 10 cm × 2 mm), and iPP films (1 cm × 13 cm × 0.5 mm) were carefully mounted at the center of block copolymer film, sandwiching it between PS and iPP. The trilayer was placed between two 2.5 mm thick stainless steal bars with Teflon sheets covering both the top and bottom surfaces and pressed at 180 °C and 1000 lb for 5 min and quenched by transferring to a second press held at 20 °C. 90° peel tests were conducted using an Instron 5966 Universal Testing System equipped with a Model 2820–035 90° Peel Test Fixture at a peel displacement speed of 10 mm/min. The peel strength was calculated by dividing the peeling force with the width of the iPP film (1 cm). People involved with sample collection, processing, analysis and/or submission: Daun Jeong - collection, processing and analysis of all data Shuquan Cui - collection of partial TEM data Nusrat Jahan - collection of high-temperature SEC data Christopher J. Ellison - analysis of data Frank S. Bates - analysis of data