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.

Optimized sustainable procedures in both acidic and basic conditions are considered to meet some of the current environmental challenges of the scientific community. In this paper, the successful syntheses of two classes of indium-based silica nanomaterials are reported. Both procedures were conceived to enhance the sustainability of the synthesis methods and promote their preparations at room temperature while avoiding the hydrothermal treatment under static conditions at 100 °C. A fast, room-temperature synthesis of porous nanospheres was conceived together with an “acid-free” procedure for SBA-15-like materials. Moreover, the isomorphic substitution of silicon with indium was achieved. All the materials were deeply characterized to probe their structural, textural and morphological properties (e.g., transmission electron microscopy, N₂ physisorption, ss MAS NMR of ²⁹Si). The high specific surface area and the mesoporosity were always preserved even under the mild reaction conditions employed. The honeycomb structure and the spherical morphology of SBA-15-like materials and nanospheres, respectively, were also observed. The insertion of indium was confirmed via X-ray photoelectron spectroscopy (XPS) investigations.

Different spectroscopies and DFT modeling have been combined to unveil the structure–activity correlation of extra-small aluminosilicate nanospheres. This study will facilitate the rational design of solid acid catalysts.