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a) CF@TiO2 b) CF@TiO2 N500 1μm 1μm c) CF@TiO2 N700 d) 1μm CF@TiO2 N900 1μm Figure 6.23. - FE-SEM images of the: a) CF@TiO2; b) CF@TiO2 N500; c) CF@TiO2 N700 d) CF@TiO2 N900. Subsequently, the XRD spectra of the samples annealed at different temperatures (Figure 6.24c) shows an initial rutile (TiO2) structure of the deposit over carbon felt with the diffraction peaks at 27.4, 35.8, and 54.38 θ, consistent with the rutile TiO2 (110), (101), and (211) crystalline planes, respectively. All peaks are in line with the standard pattern (JCPDS no.:21-1276). After the NH3-treatment at 900oC, three diffraction peaks appear at 61.8; 42.7 and, 37.2 2θ, which correspond to the (111), (200) and (220) planes of the cubic TiN phase (JCPDS: 65-0714). Below 900oC as a temperature annealing, it can only be observed a broad peak due to the nitride process at 42.7 corresponding to (210) for the rutile phase. Therefore, a more detailed analysis (Figure 6.24b) of the diffraction peaks associated with the rutile phase shows a distortion of the peak profile produced by the incorporation of nitrogen into the interstitial sites of rutile phase. i) First at all, the rutile peaks show an asymmetrical shape indicated by the area patterned with a sparse green square, as Figure 6.24b shows around 36o. It corraborates that nitride process due to the chemical interaction at the surface level is breaking TiO2 bonds producing a lattice weakness generating defects and vacancies and giving rise to a damaged outermost TiO2 layer, which justifies the asymmetrical shape of the peaks as the damaged area contributes essentially with larger interatomic distances, i.e. to the left area of the peaks212. The optical absorption capability of these defects with localized energy state in the bandgap of the material explains the color change revealed in the optical absorption spectra (Figure 6.24a). 109PDF Image | Redox Flow Batteries Vanadium to Earth Quinones
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