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a) TiN pattern CF@TiO2 N900 CF@TiO2 N700 CF@TiO2 N500 CF@ TiO2 TiO2 (rutile) pattern b) 37.24o TiN 2Theta [deg] 20 30 40 50 60 70 80 2Theta [deg] 2Theta [deg] 43.25o TiN TiO2 TiO TiO2 36o CF@TiO2 N900 CF@TiO2 N700 CF@TiO2 N500 CF@TiO2 CF@TiO2 N900 CF@TiO2 N700 CF@TiO2 N500 CF@TiO2 Figure 6.24. -. - a) X-ray diffractogram of CF@TiO2, CF@TiO2 N500, CF@TiO2 N700 and CF@TiO2 N900 electrodes, showing chacteristic TiN (top) and TiO2 (rutile, bottom) patterns. b) Detailed analysis of the XRD peaks showing the asymmetrical shape due to the nitrided process as well as the appeareance of the new TiN phase at 900oC. 6.1.3.1.2 Chemical Characterization XPS spectra analysis shows the surface effects of the nitride process. The influence of nitrogen incorporation on the state of titanium was probed through the Ti2p spectra (Figure 6.25). Significant differences can be distinguished for the CF@TiO2 N900 sample, it can be seen that 3 doublets are needed to fit the titanium signal corresponding to the different expected bonds Ti-O (458.5 eV), Ti-N-O (456.8 eV) and Ti-N (455.9 eV) in a relative percentage of 50%, 29% and 21%, respectively. Comparatively the typical TiO2 doublet related to titanium (IV) at 458.5 e eV is seen in CF@TiO2 and CF@TiO2 N500, with a small additional doublet contribution from Ti (III) in the lattice structure in case of CF@TiO2 N500 at 458.9 eV. TiN pattern CF@TiO2 N900 CF@TiO2 N700 CF@TiO2 N500 CF@TiO2 TiO2 (rutile) pattern 30 35 40 45 50 Intensity [a.u.] Intensity [a. u.] Intensity [a.u.] 41.3o 44.09o 2 Theta [deg] 2 111PDF Image | Redox Flow Batteries Vanadium to Earth Quinones
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