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Polymers 2021, 13, x FOR PEER REVIEW 12 of 15 Polymers 2021, 13, 1386 11 of 14 to the anode and second one at low frequency (i.e., 5 Hz to 100 mHz) to the cathode side [50–52]. As reported in Reference [53], the amplitude (i.e., diameter) of the low frequency side [50–52]. As reported in Reference [53], the amplitude (i.e., diameter) of the low fre- semicircle increases with the methanol concentration due to an increasing methanol cross- 0.060 0.040 0.020 0.000 2.95 3.05 3.15 3.25 3.35 1/T * 1000 (k-1) over. Similarly, in the present case, a large low-frequency semicircle indicates that, beside quency semicircle increases with the methanol concentration due to an increasing methanol the slow reaction kinetic of oxygen reduction reaction, there is a strong poisoning due to crossover. Similarly, in the present case, a large low-frequency semicircle indicates that, methanol crossover. Here, the MEA based on SPSf-SiO2_sulf shows a smaller radius for beside the slow reaction kinetic of oxygen reduction reaction, there is a strong poisoning due to methanol crossover. Here, the MEA based on SPSf-SiO _sulf shows a smaller radius the low frequency semicircle, which is translated into a lowe2r total Rp. This indicates that this membrane displays a lower methanol crossover than the other two membranes; ac- for the low frequency semicircle, which is translated into a lower total Rp. This indicates that this membrane displays a lower methanol crossover than the other two membranes; cordingly, there is a lower methanol content at the cathode, which could compete with accordingly, there is a lower methanol content at the cathode, which could compete with the oxygen reduction reaction. the oxygen reduction reaction. The same trend related to the charge transfer resistance of membranes is clearly ob- The same trend related to the charge transfer resistance of membranes is clearly served by Nyquist plots reported in Figure 6b (at 60 °C), where each radius is the sum of observed by Nyquist plots reported in Figure 6b (at 60 ◦C), where each radius is the sum of two overlapped distorted semicircles of smaller amplitude, indicating an enhanced kinetic two overlapped distorted semicircles of smaller amplitude, indicating an enhanced kinetic effect of the temperature on the reactions occurring at the cathode and anode. Addition- effect of the temperature on the reactions occurring at the cathode and anode. Additionally, ally, the values of cell resistance, obtained at high frequency intercept on the x-axis, are the values of cell resistance, obtained at high frequency intercept on the x-axis, are lower at lower at 60 °C compared with 30 °C (0.16, 0.30 and 0.48 cm2 for the MEAs based on 60 ◦C compared with 30 ◦C (0.16, 0.30 and 0.48 cm2 for the MEAs based on filler-free SPSf, filler-free SPSf, sPSf-SiO2_sulf and SPSf-SiO2, respectively). sPSf-SiO _sulf and SPSf-SiO , respectively). 22 As above reported, the conductivity of the pristine sPSf was higher than the compo- As above reported, the conductivity of the pristine sPSf was higher than the composite site membranes (Figure 7), due to the fact that the introduction of an inorganic filler, show- membranes (Figure 7), due to the fact that the introduction of an inorganic filler, showing ing very low or no proton conductivity at low temperature (30–60 °C), led to a tortuosity very low or no proton conductivity at low temperature (30–60 ◦C), led to a tortuosity increase (the same phenomenon occurring for methanol permeation, but in the case of increase (the same phenomenon occurring for methanol permeation, but in the case of protons it reduced the conductivity), causing an increase of cell resistance (see Figure 6). protons it reduced the conductivity), causing an increase of cell resistance (see Figure 6). The approach of modifying the surface characteristics of silica by sulfonation was demon- The approach of modifying the surface characteristics of silica by sulfonation was demon- strated very useful to increase the proton conductivity, allowing in the future to tailor the strated very useful to increase the proton conductivity, allowing in the future to tailor sulfonation features of the polymer to design membranes with low methanol permeability the sulfonation features of the polymer to design membranes with low methanol perme- (reducing the sulfonation degree of the polymer and using acidic functionalities on the ability (reducing the sulfonation degree of the polymer and using acidic functionalities fillers). The present results indicate that the composite membrane based on acidic silica on the fillers). The present results indicate that the composite membrane based on acidic (SPSf-SiO2_sulf) could potentially be used in high energy density DMFC devices due to a silica (SPSf-SiO2_sulf) could potentially be used in high energy density DMFC devices good compromise among low methanol crossover, low swelling due to reduced wa- due to a good compromise among low methanol crossover, low swelling due to reduced ter/MeOH uptake, good conductivity and suitable DMFC performance. water/MeOH uptake, good conductivity and suitable DMFC performance. SPSf SPSf-SiO2 SPSf-SiO2_sulf Figure 7. In-situ proton conductivity (T = 30–60 ◦C) of the different polysulfone membranes in 5 M MeOH solutions. Figure 7. In-situ proton conductivity (T = 30–60 °C) of the different polysulfone membranes in 5 M MeOH solutions. Conductivity (S cm-1)PDF Image | Properties of Methanol Transport for Direct Methanol Fuel Cells
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