Using the IR spectroscopy method, studies were carried out on the processes of hierarchical self-assembly of SiO2-SnO2 nano- and microstructures in combined sol-gel systems obtained by mixing film-forming sols with different  maturation times, which meets the goals and objectives of nanostructural engineering. Characteristic absorption peaks were identified that correspond to the process of hydrolytic polycondensation and carry information about the process of self-assembly in the analyzed systems.