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Polymers 2021, 13, 1150 12 of 14 Figure 9. Decomposition of X-ray diffraction profile near (100) Bregg peak for Li-Nafion saturated with EC/SL mixture with ω(SL) = 0.2 at the mixing temperature of 25 °C. FiguFriegu10re.A10m.oArmphoorupshaonudsacrnydstcarlylisntaelplienaekpaeraekasarfoearsLfio-NraLfii-oNnasfiaomnpslaemsbpelefosrbeeafnodreaafntedraswfterllsinwgelling with an EC/SL mixture with ω(SL) = 0.2 at different mixing temperatures (specified in the dia- with an EC/SL mixture with ω(SL) = 0.2 at different mixing temperatures (specified in the diagram). gram). Based on changes in Tg and diffraction profiles of swollen membranes, it can be asBsausmededonthcahtatnhgeepseineTtrgaatniodndoifftrhaectsionlvpenrotfiinletos othfeswamololernphmoeumsbrerganioens,siotfctahnebpeoalys-mer sumredsutlhtsatinthae pnenwetarmatoiornphoofuthsesstroulvcteunrteinthtoathinecalmudoersphnoutsornelgyiomnascorofmthoelepcoulylemsebrurte-also sultlsoiwn-amnoelwecualmaro-rwpehioguhst storluvcetnutr.eUthnaltikiencwluadters, nmootloenculylems aocfrsoomoelepcoulaers obrugtaanliscoslolwve-nts molceacnulianrt-ewraecigthwtistohlvPeFnStA. Ucnhlaikineswaantedr,pmenoeletrcautlesamofosropmheoupsolraergoiorgnasntioc wsoelvaeknetnsicnatnericnh-ain teraicnttweriatchtiPoFnSs A[4,c4h5a,5in0s]. aMndorpeoevnert,raitteisakmnowrpnhothuast rseagtuiornatsioton weitahkwenatienrtedrochesainoitnctaeurasec-any tionnso[t4ic,4e5a,b5l0e].cMhaonrgeeosvienr,thiteisNkanfiownnditfhfratcstiaotnurpartoiofinlew[4it6h].water does not cause any no- ticeable cThaenegxecseilnlenthtepNreasefirovnatdioifnfroafcatiomnepmrborfailnee[’4s6c]r.ystalline regions upon saturation with a plasticiser regardless of mixing temperature is a highly significant factor. This fact is due The excellent preservation of a membrane’s crystalline regions upon saturation with to two reasons. Firstly, the high melting point of the crystallites (≈218 ◦C) is significantly a plasticiser regardless of mixing temperature is a highly significant factor. This fact is due above the studied temperature range (25–80 ◦C). Secondly, the higher chain packing density to two reasons. Firstly, the high melting point of the crystallites (≈218 °C) is significantly of the crystalline structure makes it much more resistant to dissolution [45]. Here, the above the studied temperature range (25–80 °C). Secondly, the higher chain packing den- integrity of the membrane is ensured by crosslinking due to crystalline regions even when sity of the crystalline structure makes it much more resistant to dissolution [45]. Here, the very high degrees of swelling are achieved (>200 at 80 ◦C for EC); this also explains the integrity of the membrane is ensured by crosslinking due to crystalline regions even when apparent similarity of their characteristics with those of chemically crosslinked gels. very high degrees of swelling are achieved (>200 at 80 °C for EC); this also explains the apparent similarity of their characteristics with those of chemically crosslinked gels. 4. Conclusions Mixed solvent EC/SL is a suitable plasticiser for Li-Nafion, since it provides high 4. Conclusions −4 ionic conductivity (10 Sm cm −1 at room temperature) due to high solvent uptake. The Mixed solvent EC/SL is a suitable plasticiser for Li-Nafion, since it provides high degree of swelling of the membrane depends on the composition of the binary plasticiser and the mixing temperature; moreover, hysteresis occurs between the heating and cooling mode curves. The sorption of even small amounts of a plasticiser shifts the glass transition temperature of the ionomer from 77 ◦C to negative temperatures; at saturation with EC/SL, it decreases to below −80 ◦C. While the introduction of the plasticiser leads to the critical reorganisation of the amorphous structure of the ionomer, it does not significantly influence the crystalline regions, which remain nearly unchanged in the studied mixing temperature range of 25–80 ◦C. Due to their high melting point (about 218 ◦C), crystallites in Li-Nafion act as chemical crosslinking elements, maintaining the integrity of the membrane even at a very high solvent uptake (>200%) and making its characteristics similar to those of a chemically crosslinked gel. The obtained results provide a more in-depth insight into the physicochemical nature of the ionomer. Thus, Li-Nafion plasticised with EC/SL may be promising for use as a polymer electrolyte in developing a new generation of LIBs with enhanced safety. Author Contributions: Conceptualisation, E.A.S., Y.A.D. and O.V.B.; methodology, O.V.B.; software, T.V.Y. and O.G.R.; validation, T.V.Y., O.G.R. and L.V.S.; investigation, A.S.I., T.V.Y., O.G.R., L.V.S. and R.R.K.; data curation, L.V.S.; writing—original draft preparation, A.S.I. and O.G.R.; writing—review and editing, O.V.B.; visualisation, A.S.I., T.V.Y., O.G.R.; supervision, Y.A.D.; project administration, O.V.B.; funding acquisition, O.V.B. All authors have read and agreed to the published version of the manuscript. ionic conductivity (10−4 Sm cm−1 at room temperature) due to high solvent uptake. ThePDF Image | Li-Nafion Membrane Plasticised with Ethylene Carbonate Sulfolane
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