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Polymers 2019, 11, 914 Polymers 2018, 10, x FOR PEER REVIEW Membrane Membrane 5 of 10 5 of 10 5 of 10 (wt.%) (wt.%) (μm) Polymers 2018, 10, x FOR PEER REVIEW Table 1. Composition and thickness of the investigated membranes. Nafion TiO2-SO4 Thickness Table1.CompositionandthicknPesiscofttuherineveostifgataedtmyempbircanaesl. composite Nafion (wt.%) TiO -SO (wt.%) Thickness (μm) Picture of a typical Membrane M2 98 2 N Nafion TiO2-SO4 (wt.%1)03 ± 5(wt.%) 100107±5 2 98 Thickness Picture of a typical composite N M5 M5 M7 100 (μm) composite 24 membrane M7 93101±5 7 N 100 103 ± 5 103±5 membrane M2 98 M2 107 ±1057 ± 5 98±5 membrane 95 95 5 93 2 M5 95 5 98±5 5 98±5 7 93 7 M7 The thermal response of Nafion membranes, with and without the inorganic additive, is 101 ± 5 101±5 TheththeermrmaallrersepsopnosnesoefNofafiNoanfimonemmbreamnbesr,awneitsh, awnidthwaitnhdouwttihtheoinuotrgthaenicinaodrdgiatniviec,iasddiistpivlaey,eids °C to 280 °C, one main endothermic peak is evident, associated to an order-disorder transition of the displayed in Figure 3 in terms of DSC curves. In the temperature range under investigation, from 25 idnisFpiglauyred3iinFteigrmurseo3f iDnStCercmusrvoefsD. ISnCNthacfeuionrteviomneiscpc.lueIsnrteartsthu[2e5r]e.termanpgeruatnudrerriannvgeestuignadtieorni,nfvroemstig25atioCnt,ofr2o8m0 2C5, o°Cnetom2a8i0n °eCn,dontheemrmaiinc epnedakotihseervmidicenpte,aakssisoceivaitdeedntto, asnsocridaeter-dtisooarndeorrdtrearn-dsiitsiorndoefr thraenNsiatifioonnoifotnhiec cNluasfitoenrsi[o2n5i]c. clusters [25]. 5 0 Endo↓ 5 0 -5 -10 -15 -20 N M2 M5 M7 0 180 200 220 240 260 280 re/°C y (DSC) curves of the membranes. 4t0ran6s0itio8n0 te1m00pe1r2a0tu1r4e0 c1a6n0 b1e80at2t0r0ibu2t2e0d 2t4o0 a260wa2t8e0r-plasticizing effect, where lower transition temperatures mayTecmorprersaptuorned/ °toChigher hydration levels [28]. In our case, the change in the enthalpy values is much more important than that in Tonset. Clearly, the addition of hygroscopic sulfated titania particles causes an increase of the water content, resulting in very high ΔH values for M2 and for M5 Figure 3. Differential scanning calorimetry (DSC) curves of the membranes. with respect to plain Nafion. M7 sample, having the highest concentration of sulfated titania, apparently displays the lowest water affinity, likely due to phase segregation and non optimized Figure 3. Differential scanning calorimetry (DSC) curves of the membranes. distribution of the inorganic additive. Between all the composite membranes, M2 sample shows the The enthalpy values, derived by the DSC peaks analysis, are reported in Table 2. Those of lowest onset temperature associated to the thermal transition. composite membranes M2 and M5 are higher with respect to M7 and N samples. As explained The enthalpy values, derived by the DSC peaks analysis, are reported in Table 2. Those of −1 hydrationdegreeoftheNafionmatrix.Inparticular,M∆emHbravnealuΔHe[Jingcrea Table 2. ΔH and the Tonset associated to the DSC thermal transition of the polymer ionic clusters in the in the literature [26,27], this thermal transition, due to the polymer ionic clusters, is related to the membranes (see Figure 4). composite membranes M2 and M5 are higher with respect to M7 and N samples. As explained in the y[°Ci]ncreasing the water literature [26,27], this thermal transition, due to the polymer ionic clusters, is related to the hydration content, thanks to highly organized clusters and more cohesive interactions. At the same time, the po ly me on set N 179.29 140 ks analysis, are reported in Table 2. Those of pect to M7 and N samples. As explained in the lymer ionic clusters, is related to the hydration creases, by increasing the water content, thanks ractions. At the same time, the change in the r]sesT, b ◦◦ degreeoftheNafionmatrix.Inparticular,ΔHvalueincreaMse2s,byin2c23r.7e4asingth11e8 watercontent,thanks change in the transition temperature can be attributed to a water-plasticizing effect, where lower to highly organized clusters and more cohesive interactions. At the same time, the change in the transition temperatures may correspond to higher hydration levels [28]. In our case, the change in transition temperature can be attributed to a water-plasticizing effect, where lower transition the enthalpy values is much more important than that in Tonset. Clearly, the addition of hygroscopic temperatures may correspond to higher hydration levels [28]. In our case, the change in the enthalpy sulfated titania particles causes an increase of the water content, resulting in very high ∆H values values is much more important than that in Tonset. Clearly, the addition of hygroscopic sulfated titania for M2 and for M5 with respect to plain Nafion. M7 sample, having the highest concentration of particles causes an increase of the water content, resulting in very high ΔH values for M2 and for M5 sulfated titania, apparently displays the lowest water affinity, likely due to phase segregation and non with respect to plain Nafion. M7 sample, having the highest concentration of sulfated titania, optimized distribution of the inorganic additive. Between all the composite membranes, M2 sample apparently displays the lowest water affinity, likely due to phase segregation and non optimized shows the lowest onset temperature associated to the thermal transition. distribution of the inorganic additive. Between all the composite membranes, M2 sample shows the lowest onset temperature associated to the thermal transition. Table 2. ∆H and the Tonset associated to the DSC thermal transition of the polymer ionic clusters in the membranes (see Figure 4). membranes (see Figure 4). Membrane Membrane Table 2. ΔH and the Tonset associated to the DSC thermal transition of the polymer ionic clusters in the N M2 179.29 140 M5 223.74 118 M7 339.09 142 N M2 179.29 140 M5 339.09 142 -5 -10 -15 Endo↓ Figure 3. Differential scanning calorimetr The enthalpy values, derived by the DSCNpea M2 composite membranes M2 and M5 are higher with res literature [26,27], this thermal transition, due to the po degree of the Nafion matrix. In particular, ΔH value in to highly organized clusters and more cohesive inte 223.74 118 111.18 164 M7 Composite membranes were evaluated also in terms of water uptake (WU) and ion exchange capacity (IEC). These are important parameters because they provide a direct measure of the hydration level and of the number of available protons. Based on these parameters it possible to derived the value of λ [29]; the results are reported in Figure 4. The figure shows the composite 111.18 164 -20 40 60 80 100 120 140 16 Temperatu M5 M7 M5 339.09 142 M7 111.18 164 ∆H [J g−1polymer] ◦ ΔH [J g−1polymer] Tonset [ C] Tonset [°C] Heat flow / W g-1 Heat flow / W g -1PDF Image | Polymer Electrolyte Membranes Based on Nafion Fuel Cell
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