(Eto)(4)Si or its mixt. with (Eto)(4)Ti were hydrolyzed and polycondensed by the sot-gel method at 293 K in presence of NH3 to SiO2 or SiO2-TiO2 nanomaterials, resp. The materials were dried and studied for particle size distribution (photon spectra), structure (scanning electron microscopy, IR spectra) and elementary anal. (energy dispersive spectra). The SiO2-TiO2 nanomaterials were annealed at 550 degrees C for 5 h and tested as catalysts of ammoxidn. of cyclohexanone with NH3 and H2O2 in aq. Me3COH (pH above 8.5) to the resp. oxime. The highest selectivity (99-100%) and yield (more than 30%) of the oxime was achieved when the Ti/Si ratio in the nanocatalyst was 5.0% by mole and 7.92 % by mole.