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Effect of Composition on Polarization Hysteresis and Energy Storage Ability of P(VDF-Trfe-CFE) Relaxor Terpolymers

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Effect of Composition on Polarization Hysteresis and Energy Storage Ability of P(VDF-Trfe-CFE) Relaxor Terpolymers polymers Article Effect of Composition on Polarization Hysteresis and Energy Storage Ability of P(VDF-TrFE-CFE) Relaxor Terpolymers Yusra Hambal 1 , Vladimir V. Shvartsman 1,* , Daniil Lewin 1, Chieng Huo Huat 1, Xin Chen 2,3, Ivo Michiels 1, Qiming Zhang 2,3 and Doru C. Lupascu 1 1 Institute for Materials Science and Center for Nanointegration Duisburg-Essen (CENIDE), University of Duisburg-Essen, 45141 Essen, Germany; [email protected] (Y.H.); [email protected] (D.L.); [email protected] (C.H.H.); [email protected] (I.M.); [email protected] (D.C.L.) 2 Department of Electrical Engineering, Materials Research Institute, The Pennsylvania State University, University Park, State College, PA 16802, USA; [email protected] (X.C.); [email protected] (Q.Z.) 3 Department of Materials Science and Engineering, Materials Research Institute, The Pennsylvania State University, University Park, State College, PA 16802, USA * Correspondence: [email protected] Abstract: The temperature dependence of the dielectric permittivity and polarization hysteresis loops of P(VDF-TrFE-CFE) polymer films with different compositions are studied. Among them, the three compositions, 51.3/48.7/6.2, 59.8/40.2/7.3, and 70/30/8.1, are characterized for the first time. Relaxor behavior is confirmed for all studied samples. Increasing the CFE content results in lowering the freezing temperature and stabilizes the ergodic relaxor state. The observed double hysteresis loops are related to the field-induced transition to a ferroelectric state. The critical field corresponding Citation: Hambal, Y.; Shvartsman, to this transition varies with the composition and temperature; it becomes larger for temperatures V.V.; Lewin, D.; Huat, C.H.; Chen, X.; far from the freezing temperature. The energy storage performance is evaluated from the analysis Michiels, I.; Zhang, Q.; Lupascu, D.C. of unipolar polarization hysteresis loops. P(VDF-TrFE-CFE) 59.8/40.2/7.3 shows the largest energy Effect of Composition on Polarization density of about 5 J·cm−3 (at the field of 200 MV·m−1) and a charge–discharge efficiency of 63%, Hysteresis and Energy Storage which iscomparable with the best literature data for the neat terpolymers. Ability of P(VDF-TrFE-CFE) Relaxor Terpolymers. Polymers 2021, 13, 1343. Keywords: polymers; relaxors; energy storage; P(VDF-TrFE-CFE) https://doi.org/10.3390/polym 13081343 Academic Editor: Alexey Bubnov 1. Introduction Received: 23 March 2021 Alternative technologies in the energy generation sector, miniaturization in the elec- Accepted: 18 April 2021 tronics industry, and electric mobility have opened up many doors for advancements Published: 20 April 2021 in the field of energy storage [1]. Due to the high dielectric strength, various dielectric polymers, such as polypropylene, polycarbonate, and polyethylene terephthalate, were Publisher’s Note: MDPI stays neutral commercially used for decades in thin film and thick film capacitors, all showing a linear with regard to jurisdictional claims in dielectric response and thus a plain capacitive behavior [2–4]. For a non-linear or hysteretic published maps and institutional affil- material, the stored energy density in a polarization–electric field graph is given by the iations. area between the charging branch of a dielectric displacement—electric field hysteresis loop and the dielectric displacement axis (Figure1). Z Dmax ! ! ! Ustored = E (D)·dD, (1) Copyright: © 2021 by the authors. 0 Licensee MDPI, Basel, Switzerland. ! This article is an open access article with the dielectric displacement given by the polarization P of the material and the ! ! ! ! distributed under the terms and dielectric permittivity of free space D = #0·E + P(E). conditions of the Creative Commons Attribution (CC BY) license (https:// creativecommons.org/licenses/by/ 4.0/). Polymers 2021, 13, 1343. https://doi.org/10.3390/polym13081343 https://www.mdpi.com/journal/polymers Polymers 2021, 13, x FOR PEER REVIEW 2 of 13 storage applications [5–8]. Ideally, all this stored energy should berecoverable, which en- tails that a remanent contribution to polarization should be small. In ferroelectric poly- mers, saturation and remanent polarization often do not differ much, which is unfavora- ble for the recoverable energy storage density which is defined by the area between the discharging part of the D–E hysteresis loop and the dielectric displacement axis. = ⃗ (⃗)·⃗ (2) Therefore, materials with a high polarizability and a slim hysteresis loop are more Polymers 2021, 13, 1343 suited for energy storage applications. Such a combination of properties is typical for re- 2 of 12 laxor ferroelectrics or shortly speaking relaxors [9]. 8 Pmax. 6 Udischarged 4 Polarization (µC/cm²) Polarization 2 Prem. 0 050100 Electric Field (MV/m) Figure 1.Figure A unipolar 1. A unipolarpolarization polarization hysteresis hysteresis loop. The loop. green The area green corresponds area corresponds to the recoverable to the recoverable energy density.energy density.The hatched The hatched area yiel areads losses yields in losses the storage in the storageprocess. process. In relaxors,Therefore, the transition polymers into exhibiting a long-range high polarizabilityordered ferroelectric such as ferroelectricstate is hindered polyvinylidene by structuralfluoride or charge P(VDF) disorder.Therefore, and its copolymers polariza withtion trifluoroethylene is correlated at (TrFE), the local hexafluoropropylene scale within polar nanoregions(HFP), chlorofluoroethylene (PNRs) having asize (CFE), of a and few chlorotrifluoroethylenenanometers [9]. At high (CTFE),temperatures, as well the as blends dipole betweenmoments themof these or with PNRs other are lineardynamic dielectric and are polymers, easily rotated were studiedby an electric for energy field, storage facilitatingaapplications large polarizability [5–8]. Ideally, of relaxors. all this storedWhen energythe field should is removed, berecoverable, the PNRs whichreturn entails to a disorderedthat a remanent state, resulting contribution in a small to polarization remanent polarization. should be small. To distinguish In ferroelectric from the polymers, paraelectricsaturation state, andthis remanentstate is also polarization called the oftenergodic do notrelaxor differ state. much, which is unfavorable for the In recoverableorder to achieve energy relaxor storage behavior density which in P(VDF-TrFE) is defined by co-polymers, the area between various the dischargingtech- niques,part such of as the electron D–E hysteresis beam and loop γ-beam and theirradiation, dielectric mechanical displacement stretching, axis. and defect modification were implemented. By defect modification, another bulky monomer such as Z Dmax ! ! ! chlorofluoroethylene (CFE), hexafluoropropyleneUdischarged = (HFP),E (D )or·d Dchlorotrifluoroethylene (2) (CTFE) is incorporated into P(VDF-TrFE) [10–13].Drem It was reported that terpolymers P(VDF-TrFE-CFE)Therefore, with materials the VDF/TrFE with amolar high polarizabilityratio below 75/25 and and a slim the hysteresis molar amount loop areof more CFE > 4suited mol% forexhibit energy relaxor storage behavior applications. with a broad Such and a combination frequency-dependent of properties peakof is typicalthe for dielectricrelaxor permittivity ferroelectrics [10,11,14]. or shortly For speakingP(VDF-TrFE-CFE), relaxors [9 ].both single hysteresis loops (SHL) [15] [16],In relaxors, which are the transitiontypical for into relaxo a long-rangers, and double ordered hysteresis ferroelectric loops state (DHL) is hindered [12] by were reported.structural The or DHL charge behavior disorder.Therefore, was attributed polarization to a field-induced is correlated phase at transition. the local scale The within double polarhysteresis nanoregions behavior (PNRs) of the polymer having asizerelaxors of ais few not nanometerswell-understood [9]. At yet high [17]. temperatures, It was shown thethat dipole both SHL moments and DHL of these behavior PNRs can are be dynamic observed and in are the easily same rotated polymer by composi- an electric field, tion dependingfacilitatinga on the large synthesis polarizability conditions of relaxors. [13]. When the field is removed, the PNRs return Smallto a remanent disordered polarization state, resulting and inslim a small hysteresis remanent make polarization. P(VDFx-TrFE To1-x-CFE distinguishy) terpol- from the ymers attractiveparaelectric for state, energy this storage state is applications also called the [18,19]. ergodic A large relaxor electrocaloric state. effect was In order to achieve relaxor behavior in P(VDF-TrFE) co-polymers, various techniques, such as electron beam and γ-beam irradiation, mechanical stretching, and defect mod- ification were implemented. By defect modification, another bulky monomer such as chlorofluoroethylene (CFE), hexafluoropropylene (HFP), or chlorotrifluoroethylene (CTFE) is incorporated into P(VDF-TrFE) [10–13]. It was reported that terpolymers P(VDF-TrFE- CFE) with the VDF/TrFE molar ratio below 75/25 and the molar amount of CFE > 4 mol% exhibit relaxor behavior with a broad and frequency-dependent peakof the dielectric permittivity [10,11,14]. For P(VDF-TrFE-CFE), both single hysteresis loops (SHL) [15,16], which are typical for relaxors, and double hysteresis loops (DHL) [12] were reported. The DHL behavior was attributed to a field-induced phase transition. The double hysteresis behavior of the polymer relaxors is not well-understood yet [17]. It was shown that both Polymers 2021, 13, 1343 3 of 12 SHL
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