Mechanochemical modification of low-dispersed SnO₂ and high-dispersed SnO(OH)₂ powders with specific surface area 6 and 198 m²g⁻¹ have been studied. The crystal, porous, and electronic structure of obtained products, as well as their photocatalytic activity under visible light in the process of dyes degradation has been investigated. It has been established that high-dispersed powder is porous and poorly crystalline. Its specific surface area decreases after milling. On the contrary, low-dispersed powder is almost nonporous and well crystallized. Its specific surface area increases but degree of crystallinity reduces as a result of milling. Milling of both powders in water leads to formation of meso-macroporous structure. The narrowing of band gap and increase of adsorption of visible light occur after modification of low-dispersed sample. As a result, photocatalytic activity of milled powders under visible irradiation significantly increases. Maximal activity showed high-dispersed sample milled in air and water.

The formation of hierarchical, multimodal porosity materials with controlled shape and size of pores is the essential challenge in materials science. Properties of silica materials depend largely on different features: crystal structure, dispersity, surface composition, and porosity as well as the method of preparation and possible modification. In this paper, multimodal silicas obtained using different additives are presented. A-50 and A-380 aerosils and wide-porous SiO₂ milled at 300 rpm were used as the additives in the sol stage at 20 °C, the sol–gel stage followed by hydrothermal modification (HTT) at 200 °C, or in the mechanochemical treatment (MChT) process. The characterizations were made by application of N₂ adsorption/desorption, SEM imaging, quasi-isothermal thermogravimetry (Q-TG), dynamic thermogravimetry/derivative thermogravimetry/differential thermal analysis (TG/DTG/DTA), and cryoporometry differential scanning calorimetry (DSC) methods. Results showed that such a one-step preparation method is convenient and makes it possible to obtain multimodal silicas of differentiated porous structures and surface chemistry.