<p>This study investigates the morphology of nickel and cobalt oxides deposited on various substrates, specifically γ-alumina and silica gel. The primary objective of this study was to examine the influence of synthesis methods, such as impregnation and mechanochemical synthesis, on the textural properties and surface morphology of the resulting composites. We employed scanning electron microscopy (SEM), energy-dispersive x-ray spectroscopy (EDS), and low-temperature nitrogen adsorption/desorption (the Brunauer–Emmett–Teller (BET) method) to analyze the characteristics of the composites. The findings of the study demonstrated that the synthesis method significantly affects the particle size and shape of the oxides, as well as the distribution of nickel and cobalt oxides on the substrate surfaces. Although the impregnation method ensures a uniform distribution of metal oxide particles, they exhibit a higher tendency for agglomeration, particularly in the case of cobalt oxide. The mechanochemical method enhances the mobility of components and improves adhesion, resulting in a higher dispersion of the metal oxides. This is achieved through controlled encapsulation of the oxides within the substrate. The findings may facilitate the development of novel composite materials with improved catalytic and structural properties.</p>