N-doped TiO 2 (anatase) with high visible light photoactivity was obtained by the thermal treatment of nanotube titanic acid (denoted as NTA) in an NH 3 flow and investigated by means of X-ray diffraction (XRD), transmission electronic microscopy (TEM), diffuse reflectance spectra (DRS), X-ray photoelectron spectroscopy (XPS), electron spin resonance (ESR), and photoluminescence (PL). With increasing NH 3 treatment temperature at T = 400 to 600 1C, the anatase crystallinity of the N-NTA(400-600) samples was gradually enhanced, while at 700 1C a new phase, TiN, appeared in the N-NTA(700) sample. XPS results show that the doped N atoms incorporated into anatase TiO 2 exist in the form of NO. A revised explanation for the triplet ESR signals obtained from the N-NTA(500-700) samples was put forward, i.e. the g = 2.004 main peak is contributed by single-electron-trapped oxygen vacancies (denoted as V o ), while two weak peaks (g = 2.023, 1.987) are contributed by chemisorbed NO in well-crystallized anatase TiO 2 .The visible light photoactivity is proportional to the height of the g = 2.004 main peak, which suggests that the photoactive centers are V o -NO-Ti. The adsorbed NO molecule can effectively suppress the photoluminescence of V o defects, which facilitates photogenerated charge transfer to the surface reactive centers to conduct redox reactions. The higher the V o -NO-Ti concentration, the better the visible light photoactivity. The highest photoactivity was obtained for the catalyst, NH 3 -treated at 600 1C. But the formation of TiN at T = 700 1C can readily destruct V o -NO-Ti photoactive centers, and thus readily decreases photoactivity efficiency.
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