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Materials 2021, 14, 1617 9 of 20 Materials 2021, 14, x FOR PEER REVIEW 9 of 20 FFigiguurere4.4.AArrhrheneinuisusplpoltootfopfrportotnocnocnodnudcutivctiitvieistioesf foufllfyulhlydhryadterdatcerdoscsr-olisnsk-elidnkdeibdlodcikbliocnkomioenromer meembbrarnaenseasnadndNaNfiaofnio1n171.17. Table 3. Activation energies of cross-linked diblock ionomer membranes. A Nafion 117 membrane is The activation energies calculated from the Arrhenius plots of proton conductivity included for comparison. (Figure 4) are summarized in Table 3. The values for the cross-linked diblock ionomer membranes are all in the range of 0.076–0.095 eV; similar to the activation energy of Nafion Activation Energy 117(0.08M5emVbrmaneeasured).Activationenergyiscommonlyusedtodeducethedominant (J/mole) (eV) mechanism for proton transport. For Nafion membranes the Grotthus mechanism is dom- A50 G4 S-10 9203.6 0.095 inant if the activation energy falls within the range of 0.09–0.012 eV) [19,20]. Hence, the A100 G4 S-10 8688.1 0.090 activation energy similar to that of proton transport in Nafion may be used to infer the A150 G4 S-10 7299.7 0.076 predomiNnanfiocne 1o1f7the Grotthus mechan8is1m81.8in the diblock ionomer m0.e0m85branes. This could in turn be related to the structure and distribution of the proton transport channels, such 3a.2s.tEhxeadmoinmataioin-obfoLuiqnudidarUypsttarkuecatnudrDeiamsesnhsoiownanlSbtealboilwitybytheelectronmicrographs. Dimensional stability against liquid swelling is an important factor to consider in Table 3. Activation energies of cross-linked diblock ionomer membranes. A Nafion 117 membrane the fabrication of MEAs. Excessive membrane swelling due to a high liquid uptake can is included for comparison. cause significant changes in the membrane dimensions that lead to the deconstruction of the MEA structure. A classic failure mode is the delamination of the catalyst layers from the membrane layer resulting in poor or no fuel cell performance. Delamination indicates 0.090 Figure 5 shows the liquid uptake of the cross-linked P(AN-co-GMA)-b-SPM diblock A150G4S-10 7299.7 0.076 Membrane Activation Energy poor interfacial adhesion between the electrodes and the PEM in a MEA. This problem is commonAin50Ghy4Sd-r1o0carbon-based PEMs where m92a0t3e.r6ial properties can be signifi0c.0a9n5tly different from those of Nafion which is used as a binder in the electrodes. A100G4S-10 8688.1 ionomer membranes in comparison with the Nafion 117 membrane. Relative to the latter, the cross-linked diblock ionomer membranes had higher water uptake but lower alcohol (methanol and ethanol) uptakes. The higher water uptake could be attributed to the strong 3.2. Examination of Liquid Uptake and Dimensional Stability (J/mole) (eV) Nafion 117 8181.8 0.085 hydrophilicity of the sulfonic acid group in SPM and hydrophilicity of the –OH and –NH– groupDsinmtehnesciovnaalelnstacbroilsist-yliangkas.inAsmtloiqnguitdheswdieblloicnkgmiseamnbirmanpeos,rwtaantterfaucptotarkteoicnocrnesaisdeedrinthe wfaitbhridceactrieoansionfgMhyEdArosp.Ehoxbceics/shivyedmropemhilbicrarnateios.wTehlilsinisgidnduiecattoioanhoifgtheliqchuaindguepstinakweactaenr cause affinity which resulted in more severe membrane swelling. significant changes in the membrane dimensions that lead to the deconstruction of the In addition, the liquid uptake was also dependent on the type of alcohol solutions. MEA structure. A classic failure mode is the delamination of the catalyst layers from the Specifically, methanol uptake was much lower than ethanol uptake. This is because relative membrane layer resulting in poor or no fuel cell performance. Delamination indicates to methanol, ethanol has a solubility parameter (δ) which is closer to the solubility parame- poor interfacial adhesion between the electrodes and the PEM in a MEA. This problem is ters of most hydrocarbon monomer units (e.g., styrenic, acrylic, halide, and aromatic), and common in hydrocarbon-based PEMs where material properties can be significantly dif- hence it can better solvate the hydrophobic segments. In addition, the reduced swelling ferent from those of Nafion which is used as a binder in the electrodes. of the cross-linked diblock membranes in alcohol solutions was expected, considering the Figure 5 shows the liquid uptake of the cross-linked P(AN-co-GMA)-b-SPM diblock poor solubility of acrylic polymers such as PAN (solubility parameter, δ = 12.7) and MMA ionomer membranes in comparison with the Nafion 117 membrane. Relative to the latter, (δ = 9.5) in both methanol (δ = 7.4) and ethanol (δ = 9.5) [21]. Indeed, the extremely low the cross-linked diblock ionomer membranes had higher water uptake but lower alcohol (methanol and ethanol) uptakes. The higher water uptake could be attributed to the strong hydrophilicity of the sulfonic acid group in SPM and hydrophilicity of the –OH and –NH–PDF Image | Hydrophilic Cross-Linked Aliphatic Hydrocarbon Diblock Copolymer
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