SiO2@PDMS and CeO2–ZrO2–SiO2@PDMS nanocomposites were prepared and studied using nitrogen adsorption–desorption, Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), measurements of advancing and receding contact angles with water, and microcalorimetry. The pore size distributions indicate that the textural characteristics change after oxide modification by poly(dimethylsiloxane) (PDMS). Composites are characterized by mainly mesoporosity and macroporosity of aggregates of oxide nanoparticles or oxide@PDMS nanoparticles and their agglomerates. The FT-IR spectra show that PDMS molecules cover well the oxide surface, since the intensity of the band of free silanols at 3748 cm−1 decreases with increasing PDMS concentration and it is absent in the IR spectrum at C PDMS ≥ 20 wt% that occurs due to the hydrogen bonding of the PDMS molecules to the surface hydroxyls. SEM images reveal that the inter-particle voids are gradually filled and aggregates are re-arranged and increase from 20 to 200 nm in size with the increasing polymer concentration. The highest hydrophobicity (contact angle θ = 140° at C PDMS = 20–40 wt%) is obtained for the CeO2–ZrO2–SiO2@PDMS nanocomposites. The heat of composite immersion in water shows a tendency to decrease with increasing PDMS concentration.

A series of TiO2–ZrO2/SiO2 nanocomposites were synthesized using a liquid-phase method and characterized by various techniques, namely, nitrogen adsorption–desorption, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, high-resolution transmission electron microscopy, and photon correlation spectroscopy (PCS). It was revealed that the component ratio and calcination temperature affect the phase composition of nanocomposites. Composites TiZrSi1 (TiO2:ZrO2:SiO2 = 3:10:87) and TiZrSi2 (10:10:80) calcined at 1100 °С demonstrate the presence of t-ZrO2 crystallites in TiZrSi1 and ZrTiO4 phase in TiZrSi2. The samples calcined at 550 °С were amorphous as it was found from XRD data. According to the Raman spectra, the bands specific for anatase are observed in TiZrSi2. According to XPS data, Zr and Ti are in the highest oxidation state (+4). Textural analysis shows that initial silica is mainly meso/macroporous, but composites are mainly macroporous. The particle size distributions in aqueous media showed a tendency of increasing particle size with increasing TiO2 content in the composites.