Quantitative characterization of crystallinity in semi-crystalline fluoropolymer through 19F LF-NMR relaxometry

Crystallinity is important to the properties of a semi-crystalline fluoropolymer, such as solubility, mechanical property, bonding strength, etc. This study extended the use of 19F Low-Field Nuclear Magnetic Resonance (19F LF-NMR) to the measurement of crystallinity in the semi-crystalline fluoropol...

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Main Authors: Zhangyu Wu, Xianru He, Chunhua Zhu, Huaisong Yong, Xueyan Zhao
Format: Article
Language:English
Published: Elsevier 2024-12-01
Series:Polymer Testing
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Online Access:http://www.sciencedirect.com/science/article/pii/S0142941824003313
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author Zhangyu Wu
Xianru He
Chunhua Zhu
Huaisong Yong
Xueyan Zhao
author_facet Zhangyu Wu
Xianru He
Chunhua Zhu
Huaisong Yong
Xueyan Zhao
author_sort Zhangyu Wu
collection DOAJ
description Crystallinity is important to the properties of a semi-crystalline fluoropolymer, such as solubility, mechanical property, bonding strength, etc. This study extended the use of 19F Low-Field Nuclear Magnetic Resonance (19F LF-NMR) to the measurement of crystallinity in the semi-crystalline fluoropolymer F2314, which is the copolymer of vinylidene fluoride (VDF) and chlorotrifluoroethylene (CTFE) with a molar ratio of 1:4 and commonly used as binder in polymer-bonded explosives (PBXs). Based on the difference between spin-spin relaxometry of the 19F in crystalline region and in amorphous region, the crystallinity of F2314 can be qualitatively characterized. The obtained crystallinity exhibited a positive correlation to the time duration of thermal treatment, which is in consistent to the result of Differential Scanning Calorimetry (DSC) and X-Ray Diffraction (XRD). Moreover, 19F LF-NMR detected the slight decrease in segmental motion of crystalline region with the increase of crystallinity, and on-line monitored the evolution of segmental motion during heating. This study not only demonstrates the practicality and reliability of 19F LF-NMR in quantification of crystallinity, but also laid the foundation for in-situ characterization of fluoropolymers in PBXs in future work.
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publishDate 2024-12-01
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series Polymer Testing
spelling doaj-art-4c0b6a1672a5492085fb15aec8f38bb42025-08-20T02:38:03ZengElsevierPolymer Testing1873-23482024-12-0114110865410.1016/j.polymertesting.2024.108654Quantitative characterization of crystallinity in semi-crystalline fluoropolymer through 19F LF-NMR relaxometryZhangyu Wu0Xianru He1Chunhua Zhu2Huaisong Yong3Xueyan Zhao4Institute of Chemical Materials, China Academy of Engineering Physics, Mianyang, 621900, China; School of New Energy and Materials, Southwest Petroleum University, Chengdu, 610500, ChinaSchool of New Energy and Materials, Southwest Petroleum University, Chengdu, 610500, ChinaInstitute of Chemical Materials, China Academy of Engineering Physics, Mianyang, 621900, ChinaSchool of New Energy and Materials, Southwest Petroleum University, Chengdu, 610500, China; Department of Molecules & Materials, MESA+ Institute, University of Twente, 7500 AE, Enschede, the Netherlands; Institute Theory of Polymers, Leibniz-Institut für Polymerforschung Dresden e.V., D-01069, Dresden, Germany; Corresponding author.School of New Energy and Materials, Southwest Petroleum University, Chengdu, 610500, China.Institute of Chemical Materials, China Academy of Engineering Physics, Mianyang, 621900, China; Corresponding author.Crystallinity is important to the properties of a semi-crystalline fluoropolymer, such as solubility, mechanical property, bonding strength, etc. This study extended the use of 19F Low-Field Nuclear Magnetic Resonance (19F LF-NMR) to the measurement of crystallinity in the semi-crystalline fluoropolymer F2314, which is the copolymer of vinylidene fluoride (VDF) and chlorotrifluoroethylene (CTFE) with a molar ratio of 1:4 and commonly used as binder in polymer-bonded explosives (PBXs). Based on the difference between spin-spin relaxometry of the 19F in crystalline region and in amorphous region, the crystallinity of F2314 can be qualitatively characterized. The obtained crystallinity exhibited a positive correlation to the time duration of thermal treatment, which is in consistent to the result of Differential Scanning Calorimetry (DSC) and X-Ray Diffraction (XRD). Moreover, 19F LF-NMR detected the slight decrease in segmental motion of crystalline region with the increase of crystallinity, and on-line monitored the evolution of segmental motion during heating. This study not only demonstrates the practicality and reliability of 19F LF-NMR in quantification of crystallinity, but also laid the foundation for in-situ characterization of fluoropolymers in PBXs in future work.http://www.sciencedirect.com/science/article/pii/S0142941824003313Low-field nuclear magnetic resonanceCrystallinityFluoropolymerSpin-spin relaxometry
spellingShingle Zhangyu Wu
Xianru He
Chunhua Zhu
Huaisong Yong
Xueyan Zhao
Quantitative characterization of crystallinity in semi-crystalline fluoropolymer through 19F LF-NMR relaxometry
Polymer Testing
Low-field nuclear magnetic resonance
Crystallinity
Fluoropolymer
Spin-spin relaxometry
title Quantitative characterization of crystallinity in semi-crystalline fluoropolymer through 19F LF-NMR relaxometry
title_full Quantitative characterization of crystallinity in semi-crystalline fluoropolymer through 19F LF-NMR relaxometry
title_fullStr Quantitative characterization of crystallinity in semi-crystalline fluoropolymer through 19F LF-NMR relaxometry
title_full_unstemmed Quantitative characterization of crystallinity in semi-crystalline fluoropolymer through 19F LF-NMR relaxometry
title_short Quantitative characterization of crystallinity in semi-crystalline fluoropolymer through 19F LF-NMR relaxometry
title_sort quantitative characterization of crystallinity in semi crystalline fluoropolymer through 19f lf nmr relaxometry
topic Low-field nuclear magnetic resonance
Crystallinity
Fluoropolymer
Spin-spin relaxometry
url http://www.sciencedirect.com/science/article/pii/S0142941824003313
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AT chunhuazhu quantitativecharacterizationofcrystallinityinsemicrystallinefluoropolymerthrough19flfnmrrelaxometry
AT huaisongyong quantitativecharacterizationofcrystallinityinsemicrystallinefluoropolymerthrough19flfnmrrelaxometry
AT xueyanzhao quantitativecharacterizationofcrystallinityinsemicrystallinefluoropolymerthrough19flfnmrrelaxometry