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of graphite felt. From the fitting (Figure 6.11.b and Figure 6.11.c), can be seen that the bonding Ti-OH/Ti-O-Ti ratio significantly increases almost 150%, from 8.1 in the GF@TiO2 electrode to 19.6 in case of GF@TiO2:H. Additionally, it was observed a factor six diminution of the C-O bonding signal in the hydrogenated sample. All evidences mentioned confirm a partial reduction due to titanium dioxide oxygen deficiency as well as hydrogen absorption over the oxygen atoms linked to the Ti. 6.1.2.1.1 Electrochemical characterization Studying the electrochemical characterization of the used electrodes, It was measured the surface resistance of them using a single cell. From the I-V representation it can be obtained an initial value of 49.5 mOhm/cm2 for GF-P, which is increased when we covered with a TiO2 shell (185.2 mOhm/cm2) due to the semiconductor nature of the material. Accordingly with the XPS data treatment, the partial reduction of the shell to generate TiO2:H enhances the conductivity which is exposing as a diminution in the surface resistance (26.8 mOhm/cm2) below the initial value of pristine GF. These values are coherent with the electrochemical impedance spectroscopy (EIS) for the V3+/V2+ redox reaction happening on the electrode, showing the same behaviour (Figure 6.12). 125 100 75 50 25 0 Figure 6.12. - Cell scheme employed to measure the electrode’s electrical resistance. In order to experimentally verify the inhibition of the hydrogen-evolution reaction of the as-prepared electrodes, it was conducted linear sweep voltammetry (LSV) measurements using sulphuric acid media without vanadium electroactive ions (1M H2SO4). The current intensity obtained from these analyses corresponds to HER GF pristine GF@TiO2 GF@TiO2:H 0 25 50 75 100 125 Re(Z) / Ohm 95 -Im(R) / OhmPDF Image | Redox Flow Batteries Vanadium to Earth Quinones
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