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polymers Article Li-Nafion Membrane Plasticised with Ethylene Carbonate/Sulfolane: Influence of Mixing Temperature on the Physicochemical Properties Aigul S. Istomina 1, Tatyana V. Yaroslavtseva 1, Olga G. Reznitskikh 1, Ruslan R. Kayumov 2 , Lyubov V. Shmygleva 2, Evgeny A. Sanginov 2, Yury A. Dobrovolsky 2 and Olga V. Bushkova 1,* Citation: Istomina,A.S.; Yaroslavtseva, T.V.; Reznitskikh, O.G.; Kayumov, R.R.; Shmygleva, L.V.; Sanginov, E.A.; Dobrovolsky, Y.A.; Bushkova, O.V. Li-Nafion Membrane Plasticised with Ethylene Carbonate/Sulfolane: Influence of Mixing Temperature on the Physicochemical Properties. Polymers 2021,13,1150. https://doi.org/ 10.3390/polym13071150 Academic Editor: Srabanti Ghosh Received: 27 February 2021 Accepted: 2 April 2021 Published: 3 April 2021 Publisher’s Note: MDPI stays neutral with regard to jurisdictional claims in published maps and institutional affil- iations. Copyright: © 2021 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https:// creativecommons.org/licenses/by/ 4.0/). 1 2 * Correspondence: bushkova@ihim.uran.ru or ovbushkova@rambler.ru; Tel.: +7-343-362-3036 Abstract: The use of dipolar aprotic solvents to swell lithiated Nafion ionomer membranes simulta- neously serving as electrolyte and separator is of great interest for lithium battery applications. This work attempts to gain an insight into the physicochemical nature of a Li-Nafion ionomer material whose phase-separated nanostructure has been enhanced with a binary plasticiser comprising non- volatile high-boiling ethylene carbonate (EC) and sulfolane (SL). Gravimetric studies evaluating the influence both of mixing temperature (25 to 80 ◦C) and plasticiser composition (EC/SL ratio) on the solvent uptake of Li-Nafion revealed a hysteresis between heating and cooling modes. Differential scanning calorimetry (DSC) and wide-angle X-ray diffraction (WAXD) revealed that the saturation of a Nafion membrane with such a plasticiser led to a re-organisation of its amorphous structure, with crystalline regions remaining practically unchanged. Regardless of mixing temperature, the preservation of crystallites upon swelling is critical due to ionomer crosslinking provided by crys- talline regions, which ensures membrane integrity even at very high solvent uptake (≈200% at a mixing temperature of 80 ◦C). The physicochemical properties of a swollen membrane have much in common with those of a chemically crosslinked polymer gel. The conductivity of ≈10−4 S cm−1 demonstrated by Li-Nafion membranes saturated with EC/SL at room temperature is promising for various practical applications. Keywords: lithiated Nafion; ethylene carbonate; sulfolane; swelling; X-ray diffraction; differential scanning calorimetry 1. Introduction Along with its analogues (such as Flemion (Asahi Glass), Fumapem (Dow Chemi- cal, 3M, FuMA-Tech), Aquivion (Solvay), etc.), the perfluorinated sulfonic-acid (PFSA) ionomer Nafion® developed by DuPont in the 1960s is widely used in polymer electrolyte membrane fuel cells, sensors, vanadium flow batteries, ionistors, as well as various other electrochemical devices and electrochemical technologies [1–3]. The widespread applica- tionsofthisionomermaterialareduetoitsexcellenttransportproperties,highthermaland chemical stability, combined with stable mechanical behaviour. Ion exchange reactions can be used to convert PFSA ionomers from their original acid form to a salt form using various cations without loss of strength or thermal and chemical stability [4–14]. These properties allow PFSA salts to be used as polymer electrolytes with unipolar cation conductivity. Single-ion cationic transfer eliminates the concentration gradient in an electrochemical cell along with its problematic consequences [15,16]. At present, the lithium form of the mem- The Institute of Solid-State Chemistry, Ural Branch of the Russian Academy of Sciences, 620990 Ekaterinburg, Russia; istomina@ihim.uran.ru (A.S.I.); yaroslavtseva@ihim.uran.ru (T.V.Y.); olgarezn@ihim.uran.ru (O.G.R.) The Institute of Problems of Chemical Physics, Russian Academy of Sciences, 142432 Chernogolovka, Russia; kayumov@icp.ac.ru (R.R.K.); shmygleva@icp.ac.ru (L.V.S.); sanginov@icp.ac.ru (E.A.S.); dobr@icp.ac.ru (Y.A.D.) Polymers 2021, 13, 1150. https://doi.org/10.3390/polym13071150 https://www.mdpi.com/journal/polymersPDF Image | Li-Nafion Membrane Plasticised with Ethylene Carbonate Sulfolane
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