In this work, we investigated the kinetic balance between ammonia-catalyzed hydrolysis of tetraethyl orthosilicate (TEOS) and subsequent condensation over the growth of silica particles in the Stöber method. Our results reveal that, at the initial stage, the reaction is dictated by TEOS hydrolysis to form silanol monomers, which is denoted as pathway I and is responsible for nucleation and growth of small silica particles via condensation of neighboring silanol monomers and siloxane network clusters derived thereafter. Afterward, the reaction is dictated by condensation of newly formed silanol monomers onto the earlier formed silica particles, which is denoted as pathway II and is responsible for the enlargement in size of silica particles. When TEOS hydrolysis is significantly promoted, either at high ammonia concentration (≥0.95 M) or at low ammonia concentration in the presence of LiOH as secondary catalyst, temporal separation of pathways I and II makes the Stöber method reminiscent of in situ seeded growth. This knowledge advance enables us not only to reconcile the most prevailing aggregation-only and monomer-addition models in literature into one consistent framework to interpret the Stöber process but also to grow monodisperse silica particles with sizes in the range 15-230 nm simply but precisely regulated by the ammonia concentration with the aid of LiOH.
TiO 2 doped by different contents of indium was prepared by the sol-gel method by using titanium(IV) tetrabutoxide and indium chloride as precursors. It was revealed that a unique chemical species, O-In-Cl x (x ) 1 or 2), existed on the surface of the indium doped TiO 2 . The surface state energy level attributed to the surface O-In-Cl x species was located at 0.3 eV below the conduction band of TiO 2 . The transition of electrons from the valence band of TiO 2 to the surface state energy level was responsive to visible light. The photogenerated carriers generated under visible light irradiation can be efficiently separated by the surface state energy level of the O-In-Cl x species and the valence band of TiO 2 to contribute to the photocatalytic reaction. Consequently, the indium doped TiO 2 showed improved photocatalytic activity for photodegradation of 4-chlorophenol compared to pure TiO 2 under visible light irradiation.
The TiO2-N-x%WO3 composite photocatalysts were prepared by introducing WO3 into nitrogen-doped TiO2. The composite catalysts present much higher photocatalytic activity than TiO2 and nitrogen-doped TiO2 under both ultraviolet and visible light irradiation. Diffuse reflectance UV-vis spectra, XPS analysis, and IR spectra show that the coordinated nitrogen species (or N-metal-O linkages) may contribute to the visible light photocatalytic activity. WO3 coupling increases the active nitrogen species and thus enhances the visible light activity of the composite photocatalysts. The superior activity of TiO2-N-x%WO3 composite photocatalysts upon UV light irradiation can be rationalized in terms of efficient charge separation and high adsorption affinity of WO3.
Titanium dioxide nanoparticles were prepared via a photoassisted sol-gel method in which ultraviolet light irradiation was used in the preparation process of TiO2 colloid. After characterization by X-ray diffraction, X-ray absorption near-edge structure (XANES) at the Ti K-edge, laser Raman spectroscopy, X-ray photoelectron spectroscopy, and transmission electron microscopy, it was found that the amorphous titania nanoparticles prepared by a photoassisted sol-gel method can be transformed into crystalline anatase phase at lower calcination temperature compared to those prepared by a conventional sol-gel method. In addition, the particle size distribution of anatase powder samples is also affected by UV illumination on the colloid. It is suggested that UV illumination can induce the formation of oxygen vacancies on the colloid and this results in the accelerated phase transition from amorphous to anatase titania.
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