In recent years, the need for new generation and critical materials has brought the nanoscale materials to the center of modern research. In this study, the production of NiO/ZnO nanocomposite particles by sol-gel method was investigated for using in the petrochemical and energy sectors. In the initial solutions having a 0.1 M concentration prepared from the high purity nickel nitrate [Ni(NO3)2.6H2O)] and zinc nitrate [(Zn(NO3)2.6H2O] salts in mol (50:50)% and (30:70)%, NiO/ZnO nanocomposite particles were produced by the calcination process (700 °C, 2 hours) in the final step of the production process, which started with the use of different precipitation reagents (1 M NaOH; NH4OH) and chelating agent (0.1 M C6H8O7). Within the scope of structural characterization studies of NiO/ZnO nanocomposite particles: phase analysis by X-ray diffractometry (Rigaku, XRD); the size and morphology and to determine the qualitative proportions of the contained elements of the particles with scanning electron microscopy and energy dispersive spectroscopy (Jeol FEG SEM-EDS); and Fourier Transform Infrared Spectrometry (Bruker/Alpha-T) to determine the bonds that were present, was used. In the sol-gel method, the effect of the stoichiometry of the prepared starting solution and the precipitation reagent used in the production step on NiO/ZnO nanocomposite particle production were investigated.