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Polymers 2021, 13, 359 3 of 11 made, we could suggest which materials could be used in fuel cells, and which should be avoided, both for use and formation under operating conditions. 2. Materials and Methods 2.1. Chemicals Nafion resin solution, 5 wt% solution in a mixture of lower aliphatic alcohols and water (EW, 1100 g eq−1), Nafion 117 membranes (EW, 1100 g eq−1, 180 μm thickness), and other reagents were supplied by Sigma Aldrich (Milan, Italy) and used as received. Nafion NR212 membrane (EW 1100 g eq−1, 51 μm thickness) were supplied by Ion Power Inc. (New Castle, DE, USA) and subjected to thermal and chemical activation before the characterization. 2.2. Preparation of Nafion Uncrystallized Nafion resin solution was cast on a Petri dish (5 mL), evaporated in air for 24 h at RT, and then placed in an oven for 15 min at 80 ◦C to eliminate the solvent. The resulting membranes were peeled off the Petri dish and stored in P2O5 at RT [23]. 2.3. Preparation of Nafion 117 Oriented Nafion 117 membranes were placed in the apparatus previously described in [19] (Figure 1) with a metallic disc internal diameter of 7 cm. To avoid direct contact with the metal, the plaques were covered with a Teflon foil. The whole apparatus with tightened membranes was placed inside an autoclave at 120 ◦C, and in liquid water for about 48 h. The pressure in the autoclave simply arose from the vapor pressure of water at 120 ◦C (i.e., about 2 bar). In this conformation, the membrane swelling perpendicular to the surface was not allowed, and the parallel one was facilitated with the consequent transition to oriented materials. Then, the apparatus was cooled at RT and the samples were maintained in P2O5 at RT. Figure 1. (a) Photo and (b) schematic representation of the device used for the preparation of Nafion 117 oriented. 2.4. Preparation of Nafion Recast A Nafion recast membrane was fabricated through a typical solvent casting method. Briefly, 1 g of commercial Nafion perfluorinated resin solution was heated at about 60 ◦C until the complete evaporation of the solvents (water, alcohol, etc.), and then redissolved in 10 mL of Dimethylformamide (DMF) until a clear solution was obtained. Thereafter, the solution was cast on a Petri dish and placed in the oven at about 60 ◦C until it was dry. The membrane was finally subjected to thermal and chemical activations according to a standard method [28]. Briefly, for the membrane reinforcement, it was sandwiched and pressed between two Teflon plates and then placed in an oven at 155 ◦C for 15 min. Thereafter, the membrane was acid-activated by treating it with: (1) 1M HNO3 solution at 90 ◦C for 1 h to oxidize the organic impurities, (2) H2O2 (3 vol%) at 60 ◦C for 1 h toPDF Image | Morphology of Nafion-Based Membranes Affects Proton Transport
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