A set of polycrystalline TiO 2 photocatalysts loaded with various ions of transition metals (Co, Cr, Cu, Fe, Mo, V, and W) were prepared by using the wet impregnation method. The samples were characterized by using some bulk and surface techniques, namely X-ray diffraction, BET specific surface area determination, scanning electron microscopy, point of zero charge determination, and femtosecond pump-probe diffuse reflectance spectroscopy (PP-DRS). The samples were employed as catalysts for 4-nitrophenol photodegradation in aqueous suspension, used as a probe reaction. The characterization results have confirmed the difficulty to find a straightforward correlation between photoactivity and single specific properties of the powders. Diffuse reflectance measurements showed a slight shift in the band gap transition to longer wavelengths and an extension of the absorption in the visible region for almost all the doped samples. SEM observation and EDX measurements indicated a similar morphology for all the particles, and a not homogeneous distribution of the metal species onto the surface of catalyst particles. The impregnated samples revealed recombination rates always higher than that of bare TiO 2 . The photoactivity of TiO 2 was reduced by the presence of transition metal ions with the exception of W, which instead played a beneficial role. The results of femtosecond pumpprobe diffuse reflectance spectroscopy appear quite in accord with the observed photocatalytic activity only for the lowest values of electron-hole recombination rate of the samples.

Several commercial and homemade Ti02 samples were used as photocatalysts to prove that the physicochemical features as determined by the origin and preparation methods affect the photocatalytic behavior, in addition to the semiconducting properties. The photodegradation of aqueous phenol solution in Ti02 dispersion, carried out in a batch reactor, was used as a test reaction. The results show a great variability of photocatalytic behavior, and in particular it has been observed that the rutile phase is active or inactive according to the preparation conditions.

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Polycrystalline ZnO/TiO2 solids have been prepared with four different methods using home prepared TiO2 (anatase) or TiO2 (rutile) as supports and Zn(NO3)2·6H2O or Zn(CH3COO)2·2H2O as precursors for ZnO. The bulk and surface properties of the samples were investigated by means of TG-DTA, XRD, TEM, SEM-EDAX, XPS, BET surface area determination, and porosity measurements. XRD and TEM results indicate that no significant defect structures exist in any of the samples. The ZnO crystallinity and its enrichment on the surface of TiO2 particles were dependent on the preparation method. The surface areas generally decrease by increasing the amount of ZnO except when ZnO from Zn(CH3COO)2·2H2O was supported on TiO2 (rutile). The samples prepared from Zn(CH3COO)2·2H2O were more porous than those prepared from Zn(NO3)2·6H2O. This was confirmed by BET surface area determinations and SEM observations. XPS spectra indicate that the atomic ratio between OH- and O2- on the particles surface is similar for samples with the same ZnO content independent of the precursor used for the samples' preparation. Moreover a much higher segregation of ZnO was found for samples obtained by using the acetate precursor.