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electrode initially in oxygen atmosphere and afterwards in NH3(g) at 900oC for 4 hours each step. Additionally, this synthesis method does not imply toxic chemicals and is well- suited for large scale applications. The direct growth of TiO2 nanorods avoids the use of binders to immobilize the electrocatalyst which can suffer from deactivation, while favouring the direct transfer of electrons to the electrode. 3.2.1.1 Defective TiO2 Afterwards, the sample is annealed in oxygen atmosphere for 4 h at 500oC in order to remove chlorine impurities. This sample is labelled as GF@TiO2 electrode. Finally, the sample is treated in the presence of 5% hydrogen in argon atmosphere. In this case, the colour of the sample changed to blue after hydrogen thermal treatment, indicating a change in the electronic configuration of the metal oxide due to a partial reduction of it (Figure 3.2 ii). This new electrode was labelled as GF@TiO2:H. 3.2.1.2 Nitrided TiO2 Nitrided TiO2 nanorods have been directly grown over a commercial carbon felt (CF, 4 cm2 and 5 mm thickness from Mersen S.A., Spain) using a hydrothermal process reported above. Afterwards, TiO2-based electrodes were nitrided by NH3 gas at several temperatures 500, 700 and 900oC for 14 hours in order to study the reduction of the TiO2 to TiN (Figure 3.2 ii’). The samples were labelled as CF@TiO2N500, CF@TiO2N700 and CF@TiO2N900 electrode, respectively. 3.2.2 CeO2 synthesis Ceria have been directly deposit as an homogeneous 100 nm film over a plasma treated (GF-HT) commercial graphite felt (GF, 4 cm2 and 5 mm thickness from Mersen S.A., Spain) using an Atomic Layer Deposition (ALD) technique (Figure 3.3 i). The prepared samples were thermally treated under reductive conditions (Ar/H2 5% for 4h at 500oC) to allow the formation of GF@CeO2-x (Figure 3.3 ii). 46PDF Image | Redox Flow Batteries Vanadium to Earth Quinones
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