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Mesoporous TiO2 photocatalysts were prepared in ethanol media by using relatively green, template free sol-gel technique. A mild hydrothermal treatment procedure was employed to tune the pore sizes of the materials. Comprehensive techniques that include powder X-ray diffraction, diffuse reflectance spectroscopy, specific surface area analysis, electron microscopy, FT-IR, TGA, and ζ-potential measurements were used to characterize the titania materials. Porosity (pore size and pore volume) of the materials were found to be key factors for the variation in the rate of photocatalytic degradation of rhodamine B; in addition to specific surface area, and surface hydroxyl groups. An increase in porosity permits effective transport of the dye molecules resulting in an increase in the rate of the degradation in materials having larger pores. A detailed electrospray ionization-mass spectrometric (ESI-MS) study was carried out for selected materials to identify photodegraded intermediates and products formed during the degradation of rhodamine B. In addition, experiments were also carried out to understand the role of reactive oxygen species (ROS). In summary, this work provides a simple way to tune pore sizes without the use of any template and an insight into the influence of pore size for the photocatalytic degradation of rhodamine B.

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CdS incorporated Si-MCM-48 and Ti-MCM-48 cubic phased mesoporous photocatalysts were prepared by a two-step modification synthetic approach under relatively mild conditions. A highly efficient (24.8%, apparent quantum yield (AQY)) photocatalyst for visible light (λ > 400 nm) enabled solar hydrogen evolution can be realized by assembling CdS with Ti-MCM-48 cubic mesoporous materials in the absence of a noble metal co-catalyst. The photocatalytic mechanism was thoroughly investigated and demonstrated by conducting a wealth of characterization techniques such as powder X-ray diffraction (XRD), nitrogen adsorption isotherm, transmission electron microscopy (TEM), UV-visible diffuse reflectance spectroscopy (DRS), X-ray photoelectron spectroscopy (XPS), ultraviolet photoelectron spectroscopy (UVPS), atomic absorption spectroscopy (AAS), photoluminescence (PL) spectroscopy, time-resolved fluorescence emission decay, and electron paramagnetic resonance (EPR) spectroscopy studies. This work is the first to unambiguously identify the band positions of both CdS and TiO2 encapsulated in porous materials. The photocatalytic activity of the CdS incorporated Ti-MCM-48 mesoporous photocatalysts was found to be dependent on the content of both CdS and TiO2. A correlation between the electron injection efficiency and the photocatalytic activity was established as well in the CdS incorporated Ti-MCM-48 mesoporous photocatalysts.