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Polymers 2021, 13, 1150 4 of 14 where mdry and msw are weights of membrane samples before and after swelling, respec- tively. The uncertainty of W measurement did not exceed 1–1.5%. The molar uptake of solvent λ (equal to the number of solvents molecules per lithium cation) was calculated from W values using the formula: λ = (W × EW)/(Mrsolv × 100%), (2) where EW is the equivalent weight of the dried Li-Nafion samples (equal to 1106) and Mrsolv is the average molar mass of the used binary solvent. 2.4. Thermal Analysis The thermal behaviour of the samples was investigated using a DSC 214 Polyma differential scanning calorimeter (NETZSCH, Selb, Germany). A test sample was cut out of the membrane in the form of a disk, placed into a special Concavus Al pan, and hermetically sealed. The measurements were performed under dry nitrogen flow at 40 mL/min within a temperature range from −150 to 300 ◦C. The following temperature programme was used: heating to 50 ◦C and isothermal exposure (15 min) for additional homogenisation of the sample; cooling to −150 ◦C at 20 ◦C/min and isothermal exposure for 3 min; heating to 300 ◦C at 40 ◦C/min. 2.5. Wide-Angle X-ray Diffraction (WAXD) Wide-angle X-ray diffraction data were collected using a Stoe STADI-P diffractometer (Stoe, Darmstadt, Germany) at following conditions: Cu Kα radiation; 2θ = 5–90◦; rotating sample; symmetrical transmission mode. In order to prevent water contamination, the membrane sample under study was placed between two lavsan films. A baseline correction was applied to the data prior to further analysis. The measured profile was decomposed into the fundamental profiles by a least-squares fit, with Lorentz functions used to approximate each fundamental profile. The position, height, width, and area of obtained peaks were evaluated. The degree of crystallinity Xc (%) was determined for “dry” membrane samples from XRD data according to the following formula: Xc = Ac/(Aa + Ac) × 100%, (3) where Ac is the integrated area of the Bragg peak (100); Aa is the integrated area of the amorphous halo superimposed on the crystalline peak. 2.6. AC Conductivity Measurements Through-plane lithium conductivity was measured at a frequency range 1 Hz to 100 kHz using a Z-350M analyser (Elins LLC, Chernogolovka, Russia) with a potential amplitude of 10 mV. The membrane samples (10 mm in diameter) were placed between two blocking Ni electrodes within a hermetically sealed two-probe test cell and equilibrated for 24 h at 25 ◦C before measurement. The electrolyte resistance Re was determined by intercepting the high-frequency part of the impedance curve with the real axis. The specific conductivity σ of the samples was obtained as follows: σ = d/(Re × A), (4) where d and Re are the thickness and resistance of the sample, respectively; while A is the area of electrical contact. Conductivity was determined by impedance spectroscopy with an error about 10%.PDF Image | Li-Nafion Membrane Plasticised with Ethylene Carbonate Sulfolane
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