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Polymers 2021, 13, 359 5 of 11 were measured in the temperature range of 20 ◦C to 130 ◦C, measured every 20 ◦C, leaving the sample to equilibrate at each temperature for approximately 20 min. 2.7. Dynamic Mechanical Analysis DMA Dynamic Mechanical Analysis (DMA) was conducted by Metravib DMA/25 analyzer equipped with a shear jaw for films clamping (Limonest, France). A dynamic stress of amplitude of 10−4 at 1 Hz is applied on a rectangular shaped sample (width = 3 cm; height = 1 cm), in the temperature range of 25–200 ◦C, with a heating scan rate of 2 ◦C min−1. 2.8. Electrochemical Impedance Spectroscopy (EIS) A commercial four-electrode cell (BT-112, Scribner Associates Inc., Southern Pines, NC, USA) was adopted to measure the in-plane proton conductivity of the various Nafion membranes [31]. In this case, the membranes were cut into rectangular shapes of 25 mm × 10 mm. For the through-plane conductivity, the membrane was sandwiched between two disks of conductive carbon papers (d = 10.5 mm) and placed in a homemade two-electrode cell. Impedance spectra were recorded on a PGSTAT30 potentiostat/galvanostat/FRA (Metrohm Autolab B.V., Utrecht, The Netherlands) at OCV, over a frequency range between 1 Hz to 1 MHz, with an oscillating potential of about 10 mV. The resulting impedance data were analyzed by Metrohm Autolab NOVA software. From the Nyquist plot, the electrolyte resistance (R) was extracted as the high-frequency intercept on the real axis, and the ionic conductivity (σ) was calculated according to Equation (6) and reported as an average of three independent measurements: σ= L (6) RA where L is the distance between the electrodes and A is the active area. The in-plane and through-plane proton conductivities were measured as a function of the temperature, in the range of 20–120 ◦C, at 90% RH, leaving the sample to equilibrate for at least 30 min before each measurement. A humidification system (Fuel Cells Technologies, Inc Albuquerque, NM, USA) directly connected to the cell was used to finely control temperature and RH. 3. Results and Discussion 3.1. Conductivity Study (Through-Plane vs. In-Plane) To highlight any sort of anisotropy in the membrane morphology induced by the fabri- cation procedure, the various Nafion 1100 membranes were investigated by electrochemical impedance spectroscopy (EIS) by using two cell configurations, through-plane (σTP) and in- plane (σIP). Figure 2 illustrates the comparison between through-plane and in-plane proton conductivity of the PFSA membranes, in the temperature range of 20 ◦C to 120 ◦C at 90% RH. Furthermore, for the sake of comparison among the different Nafion-based mem- branes, some representative values are also reported in Table 1. In 2008, Holdcroft et al. [32] first compared the in-plane and through-plane conductivity of several Nafion membranes, demonstrating that the conductivity was clearly anisotropic in extruded samples, with the σIP higher than σTP, whereas it was isotropic in recast films. Furthermore, a strong correlation between the membrane thickness and the anisotropic degree was also observed: the discrepancy between in-plane and through-plane conductivity was lower for thicker membranes (i.e., 18% for Nafion 117) and increased for thinner membranes, such as Nafion 112, reaching a value of 32%.PDF Image | Morphology of Nafion-Based Membranes Affects Proton Transport
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