This file Data_Star-to-Bottlebrush-Rheology was updated on 2022-11-21 by Aristotelis Zografos Recommended citation for the data: Zografos, Aristotelis; All, Helena A; Chang, Alice B; Hillmyer, Marc A; Bates, Frank S. (2023). Supporting data for Star-to-bottlebrush transition in extensional and shear deformation of unentangled polymer melts. Retrieved from the Data Repository for the University of Minnesota, https://doi.org/10.13020/y7as-3w53. ------------------- GENERAL INFORMATION ------------------- Title of Dataset: Data_Star-to-Bottlebrush-Rheology Supporting Data for "Star-to-bottlebrush transition in extensional and shear deformation of unentangled polymer melts" 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 Principal Investigator Contact Information Name: Prof. Marc A. Hillmyer Institution: University of Minnesota Address: Department of Chemistry, 207 Pleasant St SE, Minneapolis, Minnesota 55455 Email: hillmyer@umn.edu Associate or Co-investigator Contact information Name: Aristotelis Zografos Institution: University of Minnesota Address: Department of Chemical Engineering and Materials Science, 421 Washington Ave SE, Minneapolis, Minnesota 55455 Email: zogra005@umn.edu Associate or Co-investigator Contact Information Name: Helena A. All Institution: University of Minnesota Address: Department of Chemistry, 207 Pleasant St SE, Minneapolis, Minnesota 55455 Email: all00002@umn.edu Associate or Co-investigator Contact Information Name: Alice B. Chang Institution: University of Minnesota Address: Department of Chemical Engineering and Materials Science, 421 Washington Ave SE, Minneapolis, Minnesota 55455 Email: NA Date of data collection (2021-06-01): Geographic location of data collection (where was data collected?): University of Minnesota Information about funding sources that supported the collection of the data: This research was supported by two grants from the National Science Foundation (NSF): the Center for Sustainable Polymers (grant CHE-1413862) and the Graduate Research Fellowship Program (DGE-1839286). 1H-NMR experiments were conducted at the University of Minnesota Nuclear Magnetic Resonance Laboratory using an instrument that is supported by the Director, National Institutes of Health (S10OD011952). The content of this work is solely the responsibility of the authors and does not necessarily represent the official views of the National Institutes of Health. Portions of this work were performed at the DuPont-Northwestern-Dow Collaborative Access Team (DND-CAT) located at Sector 5 of the Advanced Photon Source (APS). DND-CAT is supported by Northwestern University, The Dow Chemical Company, and DuPont de Nemours, Inc. 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 -------------------------- 1. Licenses/restrictions placed on the data:CC0 1.0 Universal 2. Links to publications that cite or use the data: Citation forthcoming 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 Zografos et al. "Star-to-bottlebrush transition in extensional and shear deformation of unentangled polymer melts." General Notes: Unless otherwise noted, all data corresponds to samples with side-chain degrees of polymerization (Nsc) of 72. The backbone degree of polymerization uses the acronym Nbb. Differential scanning calorimetry (DSC) and small-angle x-ray scattering (SAXS) data for each sample are given as individual .txt files. Extensional, small-amplitude oscillatory shear (SAOS), and stead-shear rheometry data are each in seperate Excel workbooks. Size-exclusion chromatography (SEC) data is in an Excel workbook. The uploaded SAOS data was shifted using Trios software (TA Instruments) and is referenced to 86 degrees celcius. All extensional and steady shear data corresponds to the temperatures indicated in Figure 8 of the corresponding manuscript. Files Contained: ChemDraw_Figure1.cdxml ChemDraw_Figure1.jpg DSC_Nbb10.txt DSC_Nbb100.txt DSC_Nbb150.txt DSC_Nbb20.txt DSC_Nbb200.txt DSC_Nbb30.txt DSC_Nbb300.txt DSC_Nbb430.txt DSC_Nbb50.txt DSC_Nbb58_Nsc25.txt DSC_Nbb70.txt Extensional Data.xlsx listmyfiles.text README.txt SAOS Data.xlsx SAXS_Nbb10.dat SAXS_Nbb110.dat SAXS_Nbb160.dat SAXS_Nbb20.dat SAXS_Nbb30.dat SAXS_Nbb330.dat SAXS_Nbb50.dat SAXS_Nbb70.dat SAX_Nbb210.dat SEC Data.xlsx Steady Shear Data.xlsx Data Arvhival Copy.zip 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: Small-Angle X-Ray Scattering (SAXS): SAXS studies were conducted at Sector 5-ID-D of the Advanced Photon Source at Argonne National Laboratories. Samples were hermetically sealed in DSC pans and pre-annealed for 18 hours at 60 Β°C. 1D-SAXS scattering traces were produced by azimuthally integrating the 2D-SAXS scattering data and calibrated with an Au-coated Si grating with 7200 lines/mm. The 1D patterns plot the scattering wavevector q = (4pi)*sin (πœƒ/2)/πœ† versus intensity, where πœƒ is the scattering angle and πœ† = 0.7293 β„« is the radiation wavelength. Differential Scanning Calorimetry (DSC): DSC measurements were made using a Mettler Toledo DSC 1 instrument under a nitrogen gas atmosphere. Samples were loaded into aluminum pans and hermetically sealed. The materials were heated to 150 Β°C and held isothermally for 12.5 min, then cooled to 25 Β°C and held isothermally for 5 min. Samples then underwent a second heating ramp to 200 Β°C. Each thermal ramp rate was 5 Β°C/min. Sample Preparation: Films for rheological measurements were made by placing each polymer between two teflon-lined aluminum foil sheets, which were then compression molded using a Wabash Genesis Series Hydraulic Press. Teflon shims were used to achieve a film thickness of 0.6 mm. Materials were processed between 85 and 95 Β°C, depending on the viscosity of the material. A 500 lbs force was applied for 2.5 min followed by a 1000 lbs force applied for 0.5 min. To avoid water absorption, all samples were stored in a desiccator before and after processing. Small Amplitude Oscillatory Shear Rheology (SAOS): All rheological measurements were obtained using an ARES-G2 Rheometer (TA Instruments). SAOS measurements were performed using an 8.0 mm parallel plate geometry with a gap of ~0.5 mm. Instrument compliance effects are assumed to be negligible due to the relatively small moduli of each material at the frequencies probed. Frequency sweeps were gathered at temperatures between 57 Β°C < T < 150 Β°C, depending on the polymer. Frequencies between 0.1 rad/s < πœ” < 100 rad/s were probed using a strain amplitude between 0.1% < Ξ³ < 10%. The strain amplitude was chosen based on results from strain amplitude sweeps at different temperatures and strain rates. Values were chosen within the limit of linear viscoelasticity. Master curves were created for each material by shifting the data to Tref = Tg + 34 Β°C using time-temperature superposition (TTS). Trios software was used to apply TTS and to differentiate material functions. Steady Shear Rheology: Experiments used an 8.0 mm cone and plate geometry with a truncation gap of 0.0528 mm. The measurements were obtained at temperatures of 80 to 110 Β°C and shear rates of 𝛾̇= 0.01 to 0.1 s-1. Multiple experiments were performed at these low shear rates to ensure linear viscoelastic behavior. In some cases, minor evidence of shear thinning is observed. For these samples, the extent of thinning is small and occurs at times greater than those associated with the extensional measurements, which means it does not influence any calculations associated with the strain hardening ratios. Uniaxial Extensional Rheology: Measurements were performed on 10 mm x 15 mm x 0.6 mm rectangular samples using an Extensional Viscosity Fixture (EVF). The measurements were performed at temperatures of 80 to 110 Β°C and Hencky strain rates πœ€Μ‡π» ≀ 10 s-1, which is the maximum rate that can be applied. Samples were deformed to a Hencky strain of πœ€π»= 4, which is roughly the maximum strain possible without wrapping the sample back onto itself. To mitigate sagging, measurements were initated quickly after loading samples. In some cases, a pre-stretching procedure was performed where the sample was extended at a rate chosen such that πœ€Μ‡π»β‰ͺ1/πœπ‘’π‘₯𝑑 . People involved with sample collection, processing, analysis and/or submission: Aristotelis Zografos - collection, processing and analysis of all data Helena All - collection, processing, and analysis of all rheology data Marc A. Hillmyer - analysis of data Frank S. Bates - analysis of data