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Polymers 2021, 13, 1150 11 of 14 used in the present study (transmission mode, see Section 2.5) allows the changes in the intensity of all three components of the complicated diffraction peak in the (100) region to be directly compared. Figure 10 presents the component intensities as a function of the mixing temperature and data for the “dry” membrane for comparison. The diagram demonstrates that the saturation with the plasticiser somewhat reduces the intensity of the crystal reflection (100) compared to the solvent-free membrane; an increase in the mixing temperature in the range of 25–80 ◦C also leads to a slight decrease in its intensity. However, the influence of the plasticiser on the state of the amorphous regions is much more significant: the proportion of the halo observed in the “dry” membrane sharply Figure 8. Wide-angle X-ray diffraction patterns for “dry” Li-Nafion and membrane samples Polymers 2021, 13, x FOR PEER REVIEFWigure 8. Wide-angle X-ray diffraction patterns for “dry” Li-Nafion and membrane samples sw12eollfe1d5 decreases (Figure 10). A new, very intense halo with a maximum at 19.1–19.4◦, which Polymers 2021, 13, x FOR PEER REVIEW 11 of 15 appeared due to the plasticiser sorption and noticeably increases with mixing temperature up to 60 ◦C does not change significantly at 80 ◦C. swelled with EC/SL mixture with ω(SL) = 0.2 at different mixing temperatures specified in the with EC/SL mixture with ω(SL) = 0.2 at different mixing temperatures specified in the figure. figure. Figure 9 shows an example of the decomposition into components of the measured profile in the region 2θ = 7–33°. As can be seen from the figure, the saturation with the plasticiser causes the appearance of a new broad peak (new amorphous halo) having a maximum at 2θ = 19.1–19.4°, which was absent in the dry membrane WAXD profile (right shoulder in Figure 8). The intensity of this peak noticeably increases with mixing temper- ature (and, accordingly, with solvent uptake; see Figure 4). Simultaneously, the intensity of the amorphous halo, which is identical to that appearing in the diffraction pattern of a “dry” membrane (Figure 5), decreases significantly. The WAXD technique used in the present study (transmission mode, see Section 2.5) allows the changes in the intensity of all three components of the complicated diffraction peak in the (100) region to be directly compared. Figure 10 presents the component intensities as a function of the mixing tem- perature and data for the “dry” membrane for comparison. The diagram demonstrates that the saturation with the plasticiser somewhat reduces the intensity of the crystal re- flection (100) compared to the solvent-free membrane; an increase in the mixing temper- ature in the range of 25–80 °C also leads to a slight decrease in its intensity. However, the influence of the plasticiser on the state of the amorphous regions is much more significant: Figure 9. Decomposition of X-ray diffraction profile near (100) Bregg peak for Li-Nafion saturated Figure 9. Decomposition of X-ray diffraction profile near (100) Bregg peak for Li-Nafion saturated the proportion of the halo observed in the “dry” membrane sharply decreases (Figure 10). with EC/SL mixture with ω(SL) = 0.2 at the mixing temperature of 25 °◦C. with EC/SL mixture with ω(SL) = 0.2 at the mixing temperature of 25 C. A new, very intense halo with a maximum at 19.1–19.4°, which appeared due to the plas- ticiser sorption and noticeably increases with mixing temperature up to 60 °C does not change significantly at 80 °C.PDF Image | Li-Nafion Membrane Plasticised with Ethylene Carbonate Sulfolane
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