Quasi-spherical undoped ZnO and Al-doped ZnO nanoparticles with different aluminum content, ranging from 0.5 to 5 at% of Al with respect to Zn, were synthesized. These nanoparticles were evaluated as photocatalysts in the photodegradation of the Rhodamine B (RhB) dye aqueous solution under UV-visible light irradiation. The undoped ZnO nanopowder annealed at 400 °C resulted in the highest degradation efficiency of ca. 81% after 4 h under green light irradiation (525 nm), in the presence of 5 mg of catalyst. The samples were characterized using ICP-OES, PXRD, TEM, FT-IR, ²⁷Al-MAS NMR, UV-Vis and steady-state PL. The effect of Al-doping on the phase structure, shape and particle size was also investigated. Additional information arose from the annealed nanomaterials under dynamic N₂ at different temperatures (400 and 550 °C). The position of aluminum in the ZnO lattice was identified by means of ²⁷Al-MAS NMR. FT-IR gave further information about the type of tetrahedral sites occupied by aluminum. Photoluminescence showed that the insertion of dopant increases the oxygen vacancies reducing the peroxide-like species responsible for photocatalysis. The annealing temperature helps increase the number of red-emitting centers up to 400 °C, while at 550 °C, the photocatalytic performance drops due to the aggregation tendency.

For this study, the synthesis of TiO₂ nanomaterials was performed via a novel sol-gel method employing titanium butoxide as a metal precursor, Pluronic F127 as a templating agent, toluene as a swelling agent, and acidic water or ethanol as the reaction solvents. The method was designed by tailoring certain reaction parameters, such as the sequence of toluene addition, magnetic stirring, the type of reaction solvent, and the calcination conditions. Analysis of the specific surface area and porosity was carried out via N₂ physisorption, whereas the morphological features of the solids were investigated via transmission electron microscopy. The crystalline structure of both the dried powders and the calcined materials was evaluated using X-ray diffraction analysis. It transpired that the different phase compositions of the solids are related to the specific synthesis medium employed. Under the adopted reaction conditions, ethanol, which was used as a reaction solvent, promoted the local arrangement of dispersed anatase particles, the specific arrangement of which does not lead to rutile transformation. Conversely, the use of water alone supported high-particle packing, evolving into a rutile phase. The photodegradation of Rhodamine B was used as a target reaction for testing the photocatalytic activity of the selected samples.

In this study, CeO₂, La₂O₃, and CeO₂-La₂O₃ mixed oxide catalysts with different Ce/La molar ratios were prepared by the soft template method and characterized by different techniques, including inductively coupled plasma atomic emission spectrometry, X-ray diffraction, N₂ physisorption, thermogravimetric analysis, and Raman and Fourier transform infrared spectroscopies. NH₃ and CO₂ adsorption microcalorimetry was also used for assessing the acid and base surface properties, respectively. The behavior of the oxides as catalysts for the dimethyl carbonate synthesis by the transesterification of propylene carbonate with methanol, at 160 °C under autogenic pressure, was studied in a stainless-steel batch reactor. The activity of the catalysts was found to increase with an increase in the basic sites density. The formation of dimethyl carbonate was favored on medium-strength and weak basic sites, while it underwent decomposition on the strong ones. Several parasitic reactions occurred during the transformation of propylene carbonate, depending on the basic and acidic features of the catalysts. A reaction pathway has been proposed on the basis of the components identified in the reaction mixture.

While synthesis‐properties‐performance correlations are being studied for organophosphonic acid grafted TiO₂, their stability and the impact of the exposure conditions on possible changes in the interfacial surface chemistry remain unexplored. Here, the impact of different ageing conditions on the evolution of the surface properties of propyl‐ and 3‐aminopropylphosphonic acid grafted mesoporous TiO₂ over a period of 2 years is reported, using solid‐state ³¹P and ¹³C NMR, ToF‐SIMS and EPR as main techniques. In humid conditions under ambient light exposure, PA grafted TiO₂ surfaces initiate and facilitate photo‐induced oxidative reactions, resulting in the formation of phosphate species and degradation of the grafted organic group with a loss of carbon content ranging from 40 to 60 wt %. By revealing its mechanism, solutions were provided to prevent degradation. This work provides valuable insights for the broad community in choosing optimal exposure/storage conditions that extend the lifetime and improve the materials′ performance, positively impacting sustainability.