This research is devoted to the study of the composition and surface morphology of extremely thin ‘spin-on glass’ films (~20–50 nm) doped with Pt and Pd compounds in concentrations depending on the ratio of precursors in TEOS-derived sols, their aging time and heat treatment temperature. Such methods as spectrophotometry in visible and ultraviolet regions, atomic force and scanning microscopy, X-ray reflectometry, X-ray phase analysis and voltammetry were used to study processes of the formation of sols and films based on them. The authors of this study defined features of sol-gel processes based on acid hydrolysis of TEOS in presence of dopants (Pt and Pd compounds) taken separately and together. It was shown that the combination of two dopants (Pt and Pd compounds) taken in the mole ratio of 1:1 increases catalytic activity of the films towards hydrogen. •The rate of hydrolysis of Pt, Pd complexes depends on their concentration in the sol.•Sol-gel silica layers doped by metallic Pd & Pt/Pd nanoparticles were obtained at RT.•The equimolar Pt/Pd ratio provides sol high sedimentary and aggregative stability.•Equimolar Pt/Pd ratio provides a high adsorption capacity of the catalytic layer.