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a) b)0 2 mV/s 0.5 0.0 -0.5 -1.0 -1.5 -2.0 2 mV/s -2 -4 I / A/g I / A/g GF-P GF-HT GF-TiO2(NPs) -6 GF-TiO2(SNRs) GF-TiO2(MNRs) GF-P GF-HT GF-TiO2(MNRs) GF-TiO2(NPs) GF-TiO2(SNRs) -8 -0.8 -0.6 -0.4 -0.2 0.0 0.2 0.4 -1.0 -0.8 -0.6 -0.4 -0.2 0.0 Ewe vs. NHE / V Ewe vs. NHE / V Figure 6.4. –. a) Cyclic voltammetry (CV) on the 5th cycle for different electrode synthesized at a 2 mV/s scan rate, in 0.05 M V3+ and 1 M H2SO4 solution as electrolyte b) Linear Sweep Voltammetry (LSV) 5th cycle for different electrode samples done at 2 mV/s scan rate, in 1 M H2SO4 solution as electrolyte. In both cases, the system was continuously purged with a nitrogen flow. Furthermore, Figure 6.4a. reveals the electrochemical characterization towards the negative side VRFB reaction. The values obtained from Table 6.2 indicate a reversibility increasing from the initial value for GF-HT electrode, which shows competition of the negative side redox reaction (V3+/V2+) and the hydrogen evolution reaction (HER). Afterwards, the activity towards the negative reaction, more especifically V3+ reduction to V2+, is reduced among cycling and therefore the HER is favored (Figure 6.5). Following, GF-TiO2 (NPs) displays a better reversibility towards vanadium reaction (lower value of ΔE and Ired/Iox ratio closer to 1) comparatively to GF-HT, as the functional groups of TiO2 catalyze the V3+/V2+ reaction. However, this functional groups of the titanium dioxide are reduced through continuous cycling, as Figure 6.5 shows. When the amount of initial precursor is increased in order to avoid the rapidly reduction of these functional groups, it is found the formation of SNRs on the surface that extend the ΔE in spite the fact that the ratio of reduced/oxidized intensity is enlarged. Finally, GF-TiO2 (MNRs) has the best electrochemical performance among the entire samples tested in this series of experiments. Moreover, the functional groups that catalyze the vanadium negative redox reactions are stable among ciclic voltammetry cycling, as seeing in Figure 6.5. Table 6.2. – Electrochemical parameters of cyclic voltammetry from Figure 6.4a. Compound GF –HT GF-TiO2(NPs) GF-TiO2(SNRs) GF-TiO2(MNRs) Eox / V -0.201 -0.200 -0.137 -0.200 Ered/V ΔE / V Ired/Iox -0.497 0.296 0.54 -0.495 0.293 0.64 -0.544 0.407 0.76 -0.472 0.272 0.79 87PDF Image | Redox Flow Batteries Vanadium to Earth Quinones
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