The modified sol–gel technique was proposed to obtain ZnO nanoparticles with the sizes of 30–70 nm. The proposed method allows obtaining ultradispersed powdery composites with high chemical homogeneity, which are highly demanded raw products for the development of new functional materials of a wide destination range. Metal nitrates were used as the metal sources, and hexamethylenetetramine and monoethanolamine were used to sol stabilization. Acetylacetone was used as complexing agent to obtain ultradispersed ZnO powders. The obtained powders were characterized by use XRD, TEM, N2 adsorption–desorption, FTIR spectroscopy, and element analysis. According to the results, it can be observed that Bi2O3 or/and NiO with particle sizes of ≤5 and 8–20 nm, respectively, are dispersed uniformly on the surface of ZnO nanoparticles with sizes of 50–70 nm. The chemical nature of the decoration was confirmed by the presence of characteristic bands in the FTIR spectra, indicated the chemical interaction between all structural elements of compositions.