Nowadays, nanostructures made on the basis of mixed oxides are of great interest for fundamental scientific and applied researches because of its potential applications, such as photo catalysts, luminophores, sensitive elements of gas sensors and vacuum sensors. The article describes nanostructural properties of NiO–Al2O3–SiO2 prepared by sol-gel method. Nanocomposites were obtained by mixing a solution of Si (OC2H5)4 (TEOS) as a SiO2 precursor with a solution containing Al (NO3)3 · 9H2O and Ni (NO3)2 · 6H2O. Ethanol was used as solvent. The gel was dried at room temperature and annealed in the 100–500 °C range. The behavior of chemical bonds is considered by using FTIR technique. Crystallization of NiO phase at 500 °C is observed in XRD patterns. Aluminum atoms are incorporated into silica matrix, which was confirmed by XRD. The amorphous structures which are desirable for next generations are formed at room temperature.