Characterization of end groups and branching structures in copolymers of vinylidene fluoride with hexafluoropropylene using multidimensional NMR spectroscopy

Twum, Eric B.; McCord, Elizabeth F.; Lyons, Donald F.; Fox, Peter; Rinaldi, Peter L.

doi:10.1016/j.eurpolymj.2013.12.006

Cited by 8 publications

(2 citation statements)

References 20 publications

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“…It is interesting to note that despite this transfer to DMC, the terpolymers synthesized in solution in DMC possessed sufficiently high molar masses to form self-standing films. Proton-terminated terpolymer chains generated by hydrogen abstraction from DMC, monomer, or polymer molecules (and in this case leading to short or long chain branching) , were also observed. The −CF 2 H chain ends appear as a complex signals located between 6.11 and 6.62 ppm and composed of the signals of both VDF- and TrFE-terminated polymer chains (i.e., −CF 2 –CH 2 –CF 2 H and −CF 2 –CHF–CF 2 H , respectively).…”

Section: Resultsmentioning

confidence: 92%

Influence of trans-1,3,3,3-Tetrafluoropropene on the Structure–Properties Relationship of VDF- and TrFE-Based Terpolymers

Soulestin

Filho²,

Ladmiral³

et al. 2017

Macromolecules

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trans-1,3,3,3-Tetrafluoropropene (1234ze) was copolymerized under free radical conditions with vinylidene fluoride (VDF) and trifluoroethylene (TrFE), for the first time, leading to statistical poly(VDF-ter-TrFE-ter-1234ze) electroactive terpolymers. The reactivity ratios of the three comonomer couples were determined (r VDF = 0.77; r TrFE = 0.32), (r VDF = 1.67; r 1234ze = 0.00), and (r TrFE = 7.56; r 1234ze = 0.00), at 48 °C, using the nonlinear fitting Mayo−Lewis method. 1234ze was shown to be regularly incorporated in the terpolymer chains over the entire course of the reaction providing terpolymer chains with statistical monomer distribution and almost constant composition. These new VDF/TrFE-based terpolymers were characterized by 1 H and 19 F liquid state NMR spectroscopy. The characteristic NMR signals of the VDF− 1234ze dyads were identified by comparing the NMR spectral signatures of a poly(VDF 82 -co-1234ze 18 ) copolymer and of a terpolymer. The thermal and electroactive properties of poly(VDF-ter-TrFEter-1234ze) terpolymers, with 1234ze content ranging from 0 to 6 mol % and molar masses above 55 kg/mol, were assessed. The randomly distributed 1234ze termonomer units induced the decreases of both the Curie and the melting temperatures of the terpolymer even at low termonomer content (T Curie = 70 °C and T m = 126 °C and T Curie = 72 °C and T m = 150 °C; for a poly(VDF 69 -ter-TrFE 28 -ter-1234ze 3 ) terpolymer and a poly(VDF 65 -co-TrFE 35 ) copolymer, respectively). Films of the terpolymers were cast, and their electroactive properties were examined by D−E loops measurements. They showed that the presence of 1234ze decreased the remnant polarization (P r = 45 mC/m 2 for a poly(VDF 65 -co-TrFE 35 ) copolymer to 28 mC/m 2 for a poly(VDF 69 -ter-TrFE 25 -ter-1234ze 6 ) terpolymer) probably because it also decreased the crystallinity of the terpolymer. The combination of the studies of the reactivity of the monomers, of the terpolymer microstructures, and of the assessment of their physical properties provides insights into their structure−property relationship.

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Section: Resultsmentioning

confidence: 92%

Influence of trans-1,3,3,3-Tetrafluoropropene on the Structure–Properties Relationship of VDF- and TrFE-Based Terpolymers

Soulestin

Filho²,

Ladmiral³

et al. 2017

Macromolecules

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“…The compositions of the elastomers can be determined by NMR spectroscopy as carefully studied by Rinaldi's team. Indeed, two interesting articles report in-depth characterizations of poly(VDF-co-HFP) copolymers [247] and poly(VDF-ter-HFP-ter-TFE) elastomers [248].…”

Section: Fluorinated Elastomersmentioning

confidence: 99%

Copolymers of vinylidene fluoride with functional comonomers and applications therefrom: Recent developments, challenges and future trends

Améduri

2022

Progress in Polymer Science

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TFE Terpolymers: Once Promising – Are There Still Perspectives in the 21st Century: Synthesis, Characterization, and Properties‐Part I

Ok,

Steinhart,

Scheler

et al. 2024

Macromol. Rapid Commun.

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Polytetrafluoroethylene (PTFE) exhibits outstanding properties such as high‐temperature stability, low surface tension, and chemical resistance against most solvents, strong acids, and bases. However, these traits make it challenging to subject PTFE to standard polymer processing procedures, such as thermoforming and hot incremental forming. While polymer processing at temperatures above the melting point of PTFE is already demanding, the typically large molar mass of PTFE results in extremely high melt viscosities, complicating the processing of PTFE. Also, PTFE tends to decompose at temperatures close to its melting point. Therefore, fluoropolymers obtained by copolymerizing tetrafluoroethylene (TFE) with various co‐monomers are studied as alternatives to PTFE (e.g., fluorinated ethylene‐propylene (FEP)), combining its advantages with better processability. TFE terpolymers have emerged as desirable PTFE alternatives. This review provides an overview of the synthesis with various comonomers and microstructural analysis of PTFE terpolymers and the relationships between the microstructures of TFE terpolymers and their properties.

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Characterization of end groups and branching structures in copolymers of vinylidene fluoride with hexafluoropropylene using multidimensional NMR spectroscopy

Cited by 8 publications

References 20 publications

Influence of trans-1,3,3,3-Tetrafluoropropene on the Structure–Properties Relationship of VDF- and TrFE-Based Terpolymers

Influence of trans-1,3,3,3-Tetrafluoropropene on the Structure–Properties Relationship of VDF- and TrFE-Based Terpolymers

Copolymers of vinylidene fluoride with functional comonomers and applications therefrom: Recent developments, challenges and future trends

TFE Terpolymers: Once Promising – Are There Still Perspectives in the 21st Century: Synthesis, Characterization, and Properties‐Part I

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