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Polymers 2021, 13, 1150 amorphous structure was observed. These results provide an insight into the physico- chemical nature of Li-Nafion membranes swollen with aprotic solvents. 2. Materials and Methods 3 of 14 2.1. Membrane Preparation In this work, a commercial Nafion® 115 (125 μm) (Du Pont de Nemours, Wilmington, 2. Materials and Methods DE, USA) extrusion membrane was used. The Li+ form of the membrane was prepared as 2.1. Membrane Preparation described in our previous work [9] and shown in Figure 2 over the course of four consec- In this work, a commercial Nafion® 115 (125 μm) (Du Pont de Nemours, Wilmington, utive stages: purification, neutralisation by LiOH, thorough washing and drying. The DE, USA) extrusion membrane was used. The Li+ form of the membrane was prepared samples were first dried in air at 60 °C for 1 h and then in a desiccator at room temperature as described in our previous work [9] and shown in Figure 2 over the course of four over P2O5 for seven days. Residual water content was monitored by infrared Fourier spec- consecutive stages: purification, neutralisation by LiOH, thorough washing and drying. troscopy (Bruker Vertex 70v, Bruker Corporation, Karlsruhe, Germany) and simultaneous The samples were first dried in air at 60 ◦C for 1 h and then in a desiccator at room thermal analysis (STA 449 F3 Jupiter, NETZSCH, Selb, Germany). temperatureoverPO forsevendays.Residualwatercontentwasmonitoredbyinfrared 25 All further manipulations of the Li-Nafion membrane and plasticisers were per- Fourier spectroscopy (Bruker Vertex 70v, Bruker Corporation, Karlsruhe, Germany) and formed in an MBRAUN UNILAB glovebox (MBraun Inertgas-Systeme, München, Ger- simultaneous thermal analysis (STA 449 F3 Jupiter, NETZSCH, Selb, Germany). many) in an argon atmosphere (the content of H2O and O2 < 1 ppm). FFigiguurere22..ScShchememeeooffththeeNNafaifioonnmmemembbraranneeliltihthiaiatitoionnpprorocecesss.. All further manipulations of the Li-Nafion membrane and plasticisers were performed 2.2. Binary Plasticiser Preparation in an MBRAUN UNILAB glovebox (MBraun Inertgas-Systeme, München, Germany) in an A binary EC/SL plasticiser was prepared from anhydrous ethylene carbonate (99%) argon atmosphere (the content of H2O and O2 < 1 ppm). and sulfolane (99%), both from Sigma Aldrich (St. Louis, MO, USA)). The mass fraction of sulfolane (ω(SL)) in the EC/SL mixtures varied from 0 to 1 with an increment of 0.05–0.10. 2.2. Binary Plasticiser Preparation Since the melting points of ethylene carbonate and sulfolane are above room temperature A binary EC/SL plasticiser was prepared from anhydrous ethylene carbonate (99%) (≈36 and ≈29 °C, respectively), they were heated until wholly melted (up to 40 °C for EC and sulfolane (99%), both from Sigma Aldrich (St. Louis, MO, USA). The mass fraction of and up to 30 °C for SL). Then, the mixtures were stirred for 30 min using a magnetic stirrer sulfolane (ω(SL)) in the EC/SL mixtures varied from 0 to 1 with an increment of 0.05–0.10. and kept at room temperature for at least 24 h before use. Since the melting points of ethylene carbonate and sulfolane are above room temperature (≈36 and ≈29 ◦C, respectively), they were heated until wholly melted (up to 40 ◦C for EC 2.3. Membrane Swelling and up to 30 ◦C for SL). Then, the mixtures were stirred for 30 min using a magnetic stirrer The swelling of the Li-Nafion membrane was investigated gravimetrically; each ex- and kept at room temperature for at least 24 h before use. periment was repeated in triplicate. A dry membrane sample was placed in an excess vol- u2m.3e.oMfesmolbvreante(SEwCe,llSinLg,orEC/SL)overactivated3Åmolecularsieves.Toachieveanequi- librium degree of swelling, the samples were held under isothermal conditions for 24 h The swelling of the Li-Nafion membrane was investigated gravimetrically; each (from 40 to 80 °C). The initial and final sample weights were measured. To remove the experiment was repeated in triplicate. A dry membrane sample was placed in an excess volume of solvent (EC, SL, or EC/SL) over activated 3Å molecular sieves. To achieve an equilibrium degree of swelling, the samples were held under isothermal conditions for 24 h (from 40 to 80 ◦C). The initial and final sample weights were measured. To remove the surface solvent, the samples were blotted dry before measurements. The weight uptake W (%) was calculated as: W = (msw − mdry)/mdry × 100%, (1)PDF Image | Li-Nafion Membrane Plasticised with Ethylene Carbonate Sulfolane
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