Polymer Crystallization Studied by Hyphenated Rheology Techniques: Rheo‐NMR, Rheo‐SAXS, and Rheo‐Microscopy

Räntzsch, Volker; Özen, Mürüvvet Begüm; Ratzsch, Karl‐Friedrich; Stellamanns, Eric; Sprung, Michael; Guthausen, Gisela; Wilhelm, Manfred

doi:10.1002/mame.201970004

Cited by 6 publications

(3 citation statements)

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“…16,17 With the continuous advancement of research and technological innovation, a growing number of researchers have redirected their focus towards investigating the evolutionary process of microstructure. Notably, some researchers have successfully achieved in situ microscopic observation by rheo-microscopy 18,19 in many elds, such as blood, 20 colloidal suspensions, 21,22 crystals, 23,24 bers, 25,26 so materials 27 and other complex multiphase system rheology and microstructure studies. Villa 28 constructed a rheo-microscopic device that combined a stress-controlled rheometer with differential dynamic microscopic analysis of particle tracking to test the advantages and limitations of the sample under test.…”

Section: Introductionmentioning

confidence: 99%

Study on microstructure evolution of waxy crude oil emulsions under dynamic cooling conditions

Dong,

Guo,

Zhang

et al. 2024

RSC Adv.

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Section: Introductionmentioning

confidence: 99%

Study on microstructure evolution of waxy crude oil emulsions under dynamic cooling conditions

Dong,

Guo,

Zhang

et al. 2024

RSC Adv.

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“…[4] Many characterization techniques have been employed to study the crystallization behavior of semicrystalline polymers by monitoring the T-dependent changes in molecular chain conformations, microstructures, and macroscopic thermal/mechanical/optical properties. They include calorimetric techniques such as conventional differential scanning calorimetry (DSC) [8][9][10] and (ultra)fast scanning calorimetry (capable of accessing high cooling rates up to ≈5000 °C s −1 ); [11][12][13][14] spectroscopic methods such as ellipsometry, UV-vis, Fouriertransform infrared (FTIR), Raman, and solid-state nuclear magnetic resonance; [15][16][17][18][19] microscopy methods such as optical microscopy, transmission or scanning electron microscopy (TEM/SEM), and atomic force microscopy (AFM); [20][21][22][23] scattering methods such as XRD, small/wide-angle X-ray scattering (SAXS/WAXS), and light/neutron scattering, [24][25][26][27][28][29][30][31] rheology, [8] and others. [32][33][34][35] Despite the promising research progress in this field, these previous techniques have their own limitations such as low sensitivity and availability in laboratorial/industrial research settings (e.g., X-ray based scattering techniques often require the use of scarce synchrotron X-ray beams in order to achieve high resolution [28] ).…”

Section: Introductionmentioning

confidence: 99%

Crystallization Behavior of Semicrystalline Polymers Characterized by an In Situ Fluorescence Technique and its Sensing Mechanism

Nile,

Feng,

Cabello

et al. 2023

Macro Chemistry & Physics

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In this study, fluorescence spectroscopy is used to study the bulk nonisothermal and isothermal crystallization of poly(L‐lactic acid) (PLLA) by monitoring in situ the temperature (T)‐ and time (t)‐dependent fluorescence intensity of the fluorophores incorporated into the PLLA matrix, respectively. The crystallization behavior characterized by fluorescence resemble those measured by conventional differential scanning calorimetry, confirming the validity of this fluorescence technique for sensing crystallization. Combined in‐situ fluorescence results and ex‐situ X‐ray diffraction characterizations demonstrate that this fluorescence technique shows great sensitivity not only to the degree of crystallinity but also to the crystalline microstructures formed during crystallization (e.g., α versus α' form PLLA crystals). Moreover, complementary fluorescence microscopy to this technique help reveal the intrinsic crystallization sensing mechanism: As crystals form during crystallization, the bulky fluorescent probes excluded from the crystalline regions reside in the rigid/mobile amorphous (i.e., non‐crystalline) regions of the resulting semicrystalline matrix, and their intramolecular motions are restricted by the neighboring crystalline domains and thus their fluorescence intensity is greatly enhanced upon crystallization. Because of its high sensitivity, fluorescence is powerful for studying the crystallization behavior of ultrathin polymer films (e.g., 75 nm) and elucidating confinement and interfacial effects through future studies.This article is protected by copyright. All rights reserved

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“…The Rheo-NMR, which combines rheometer and NMR, becomes a versatile instrument to capture the molecular-level information under shear or deformation. Most of the Rheo-NMR instruments are designed based on various shear cells, − whereas reports related to the tensile mode are quite limited . Nishi et al first investigated the chain dynamics and strain-induced crystallization of various elastomers, i.e., natural rubber, by measuring the NMR of a deformed sample with a fixed stretch ratio.…”

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confidence: 99%

Time-Resolved Extensional Rheo-NMR Spectroscopy for Investigating Polymer Nanocomposites under Deformation

Xiong

Xia

et al. 2023

Anal. Chem.

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Understanding the microstructure change of polymer nanocomposites (PNCs) under elongation deformation at the molecular level is the key to coupling structure−property relationships of PNCs. In this study, we developed our recently proposed in situ extensional rheology NMR device, Rheo-spin NMR, which can simultaneously obtain both the macroscopic stress−strain curves and the microscopic molecular information with the total sample weight of ∼6 mg. This enables us to conduct a detailed investigation of the evolution of the interfacial layer and polymer matrix in nonlinear elongational strain softening behaviors. A quantitative method is established for in situ analysis of (1) the fraction of the interfacial layer and (2) the network strand orientation distribution of the polymer matrix based on the molecular stress function model under active deformation. The results show that for the current highly filled silicone nanocomposite system, the influence of the interfacial layer fraction on mechanical property change during small amplitude deformation is quite minor, while the main role is reflected in rubber network strand reorientation. The Rheo-spin NMR device and the established analysis method are expected to facilitate the understanding of the reinforcement mechanism of PNC, which can be further applied to understand the deformation mechanism of other systems, i.e., glassy and semicrystalline polymers and the vascular tissues.

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Polymer Crystallization Studied by Hyphenated Rheology Techniques: Rheo‐NMR, Rheo‐SAXS, and Rheo‐Microscopy

Cited by 6 publications

References 0 publications

Study on microstructure evolution of waxy crude oil emulsions under dynamic cooling conditions

Study on microstructure evolution of waxy crude oil emulsions under dynamic cooling conditions

Crystallization Behavior of Semicrystalline Polymers Characterized by an In Situ Fluorescence Technique and its Sensing Mechanism

Time-Resolved Extensional Rheo-NMR Spectroscopy for Investigating Polymer Nanocomposites under Deformation

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