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Polymers 2021, 13, x FOR PEER REVIEW Polymers 2021, 13, 1150 3. Results and Discussion 5 of 15 5 of 14 3. Results and Discussion 3.1. Characterisation of the Plasticiser 3.1. Characterisation of the Plasticiser An important point in selecting EC and SL as components of the binary plasticiser An important point in selecting EC and SL as components of the binary plasticiser was the obvious similarity of their molecular structure (Figure 1b,c). Both of these solvents was the obvious similarity of their molecular structure (Figure 1b,c). Both of these solvents readily dissolve lithium salts due to the intermediate (SL) and high (EC) dielectric con- readily dissolve lithium salts due to the intermediate (SL) and high (EC) dielectric constants stants (60 and 90, respectively [27]), high dipole moment (4.93 for EC and 4.81 for SL [28]), (60 and 90, respectively [27]), high dipole moment (4.93 for EC and 4.81 for SL [28]), and the and the presence of electron donor groups capable of coordinating the lithium cation (Fig- presence of electron donor groups capable of coordinating the lithium cation (Figure 1b,c). ure 1b,c). This explains the effective solvation of Li+ in lithiated Nafion upon swelling with This explains the effective solvation of Li+ in lithiated Nafion upon swelling with EC, SL, EC, SL, or an EC/SL mixture. The combination of high boiling points with low vapour or an EC/SL mixture. The combination of high boiling points with low vapour pressure at pressure at T < 100 °C (0.003 and 0.009 kPa, respectively [29,30]) and high flash points T < 100 ◦C (0.003 and 0.009 kPa, respectively [29,30]) and high flash points (145.5 ± 4 and (145.5 ± 4 and 165 ± 4 °C [30]) offered by both EC and SL solvents is an important factor in 165 ± 4 ◦C [30]) offered by both EC and SL solvents is an important factor in improving improving the safety of LIBs. the safety of LIBs. While EC and SL solvents have individual melting points above room temperature While EC and SL solvents have individual melting points above room temperature (36.4 and 28.5 °C, respectively [28]), the mixture formed therefrom offers a significant de- (36.4 and 28.5 ◦C, respectively [28]), the mixture formed therefrom offers a significant de- crease in the melting point of the plasticiser. Indeed, as established in our recent work crease in the melting point of the plasticiser. Indeed, as established in our recent work [31], [31], the EC–SL system belongs to a simple eutectic type with a eutectic temperature of— the EC–SL system belongs to a simple eutectic type with a eutectic temperature of—16 ◦C 16 °С and a eutectic point at 70 wt % SL. Moreover, binary EC/SL mixtures in a moderate and a eutectic point at 70 wt % SL. Moreover, binary EC/SL mixtures in a moderate range range of compositions 50 to 75 wt % SL are prone to transition into the metastable state of of compositions 50 to 75 wt % SL are prone to transition into the metastable state of a a supercooled liquid without crystallisation of components (i.e., becoming glassy) [31], supercooled liquid without crystallisation of components (i.e., becoming glassy) [31], which which makes them nearly ideal plasticisers. As shown in our previous work [26], it is ad- makes them nearly ideal plasticisers. As shown in our previous work [26], it is advisable to visable to saturate membranes with ES/SL binary plasticiser at tempera◦tures ≥40 °C when saturate membranes with ES/SL binary plasticiser at temperatures ≥40 C when both EC both EC and SL components are in a liquid state. and SL components are in a liquid state. 33.2.2. .IInnflfulueenncceeooffPPlalasstitcicisiseerrCCoomppoossitiitoionnoonnSSoolvlvenenttUUpptatakkeeaannddCCoonndduuctcitvivitiyty TThheemeembbraranneesswweereresasatuturaratetdedwwitihthEECC//SSLbbiinaarryymixixttuurreessooffvvaarryyininggccoomppoosistiitoionn ◦ FFigiguurere33.. Weightuupptatakkee(W(W) )anadndmmolaorlaurputapkteak(λe)((λa)) (aan)dacnodndcounctdivuicttyivoiftyswooflslewnoLllie-Nn aLfi-oNnamfieomn - aatt4400 °CC..TThheesosolvlveennttuupptatakkeewwaassddeefifnineeddbbyyththeeggraravvimimeetrtircictetechchnniqiquueeaassddeescsrcirbibeeddinin SSeecctitoionn22.3.3. .FFiiggurree33aaililulusstrtraatteessththeeddeeppeennddeenncceeooffththeewweeigighhttuupptatakkeeW(c(acalclcuulalateteddbbyy EEqquuaatitoionn(1()1))v)sv.sω.ω(S(LS)L.)I.tcItancabnebseensetehnaththaeththigehhesigthWesvtaWluevraelluaetersetloatehsetpoutrheeECpu,wrehEilCe, thwehsiloelvthenetsuoplvteankte udpetcarkeeasdesecarseaωse(SsLa)siωnc(rSeLa)seinscfreoamses13f2ro.5m% 1(3p2u.5re%E(Cp)udreowECn)todo8w8.n1%to (p88u.r1e%SL(p).ure SL). ◦◦ brane at 25 °C (b) as a function of ω(SL) (mixing temperature of 40 °C) membrane at 25 C (b) as a function of ω(SL) (mixing temperature of 40 C). Onnththeeaasssuumpptitoionnththaattththeemmixixeeddsosolvlveennt tcocommppoossitiitoionnaabbssoorbrbeeddbbyyLLi-iN-Naafifoionnisis idideenntitcicaalltotoththeeininitiitaial lmixixtuturreeuusseedd(n(nooseselelecctitviveesosorprptitoionn),),ththeetototatal lnnuumbbeerroof fbbininaaryry pplalasstitcicisiseerrmooleleccuulelessppeerrLLi iccaattiionininththeesswoollelennLLi-iN-Naafifoionnmeembbrraanee((moollaarruupttaakeeλλ)) waassccaalclcuulalatetedduussininggEEqquuaatitoionn(2(2).). Ass ccaan bee sseeen ffrroomFFigiguurree33aa, ,ththeeWaannddλλvvaaluluees s ddeeccrereaaseserarpapididlylyasaωs ω(S(LS)Li)nicnrecaresaes,ews,hwilheitlheethλevλaluveasludeisffedriftfwerictewfoicrepfuorepsuolrveesnotlsvEeCntasnEdC SL (λ = 16.6 and 8.1, respectively). Here, it is important to note that the λ values are much and SL (λ = 16.6 and 8.1, respectively). Here, it is important to note that the λ values arePDF Image | Li-Nafion Membrane Plasticised with Ethylene Carbonate Sulfolane
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