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Polymers 2021, 13, x Polymers 2021, 13, 1258 8 of 14 (a) Figure 4. Electrostatic force microscopy (EFM) image of (a) dry and (b) wet membrane. Figure 5 depicts the line profiles of the dry and wet proton exchange membranes, providing numerical information on the phase shift at each bias voltage. Both images show small changes for a phase shift of ~0.2° when the same bias voltage is maintained, and a relatively large phase shift of 1° is observed when the bias voltage changes. Both membranes have positive phase shift values between –3 V and 0 V, indicating that the net electrostatic force between the tip and the sample surface is repulsive. In the negative bias voltage configuration, the tip is positively charged, and typically, the force between the tip and the sample surface is attractive, owing to the negatively polarized membrane surface. The result depicts the opposite phenomenon, implying that the sample surface is positively charged. For negative bias voltages, phase lag values are slightly higher for dry (am) embranes than those for wet membranes. The phase sh(ibft)is negative between 2 V and 3 V, indicating that the force is in the attractive regime. With these bias voltages, both Figure 4. Electrostatic force microscopy (EFM) image of (a) dry and (b) wet membrane. Figure 4. Electrostatic force microscopy (EFM) image of (a) dry and (b) wet membrane. membranes have similar phase lag values. Figure 5 depicts the line profiles of the dry and wet proton exchange membranes, 54 (b) 8 of 13 -3 V providing numerica show small changes and a relatively larg membranes have po 0V 4 3 l information on the ph-3aVse shift at each bias voltage. Both images for a phase shift of ~0.2° when the same bias voltage is maintained, -2 V -1 V electrostatic force be voltage configuratio tip and the sample surface. The result d positively charged. membranes than tho 3 -2 V e phase shift of 1° is observed when the bias voltage changes. Both 2 -1 V sitive phase shift values between –3 V and 0 V, indicating that the net 20V 1 0 -1 -2 0 200 5 -3V 4 tween the tip and the sample surface is repulsive. In the negative bias 1 n, the tip is positively charged, and typically,1tVhe force between the surface is attractive, owing to the negatively polarized membrane epicts the opposite phenomenon, implying that the sample surface is For negative bias volt-a1ges, phase lag values are slightly higher for dry se for wet membranes. The phase shift is negative between 2 V and 3 (b) 0 2V 800 1000 -2 V, indicating that the force is in the attractive regime. With these bias voltages, both 400 600 200 400 600 800 1000 x(nm) 3V 1 0 -1 -2 0 200 1V11V value varies linearly with bias voltage in both membranes, as shown in Figure 6. There X (nm) 0 membranes have similar phase lag values. (a) 4 -3V -2V Figure5.Lineprofileof(a)dryand(b3)wetme-2mVbrane. Figure 5. Line profile of (a) dry and (b) wet membrane. -1 V 2 -1 V 3 20V 0V X (nm) 1V 2V 3V For more detailed analysis, the mean phase value at each bias voltage was plotted for For more detailed analysis, the mean phase value at each bias voltage was plotted for both the dry and wet membranes. From the analysis, it can be observed that the phase lag both the dry and wet membranes. From the analysis, it can be observed that the phase lag arelocally2Vchargedregionsonthemem0brane,thebehaviorofwhic2hVischaracterizedby the second term3 Vin (13). As the phase lag is the sum of both terms in (13), a3 Vpositive phase -1 lag value indicates that the second term, related to the local surface charge, is dominant. When the bias voltage is reduced, the phase lag decreases. For the wet membrane, the 400 600 800 1000 -20 200 400 600 800 1000 phase lag values of 3.4◦, 2.5◦, and 1.8◦ were noted at bias voltages of −3 V, −2 V, and x(nm) −1 V, indicating that both terms in the equation decreased as the bias voltage was reduced. (aF)orthedrymembrane,thephaselagvalueswere4.0◦,(3b.)4◦,and2.5◦at−3V,−2V,and −1 V, respectively. Wet membranes typically have higher proton conductivities than dry Figure 5. Line profile of (a) dry and (b) wet membrane. membranes, and a high ionic channel network density, because of their creation of a new ionic channel network. The difference between the phase lag values of wet and dry For more detailed analysis, the mean phase value at each bias voltage was plotted for membranes is thus related to the second term in (13). At 1 V, this value is close to zero. both the dry and wet membranes. From the analysis, it can be observed that the phase lag In contrast, at 2 V and 3 V, both membranes have similar negative phase values. Both membranes have similar phase values at 2 V and 3 V. Specifically, dry and wet membranes Phase (Degree) Phase (Degree) Phase (Degree) Phase (Degree)PDF Image | Ionic Domains on a Proton Exchange Membrane Electrostatics
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