The physicochemical properties of synthetic powders depend strongly on the method of their preparation. The present work concerns the use of the sol-gel method to prepare xMgOÁySiO 2 powders with defined physicochemical and structural properties. An important objective was to determine how the basic process parameters (including the type and concentration of the reactants) influence the physicochemical properties of the resulting material. To obtain a synthetic powders, organic precursors of magnesium (magnesium ethoxide), and silicon (tetraethoxysilane) were used. Selected products were subjected to calcination to identify the crystalline structure of the powders and to determine the impact of the proposed method of preparation on this parameter. This aspect of the research will significantly improve the range of application of the manufactured products. The powders obtained by the proposed method were thoroughly analyzed in terms of chemical composition, crystalline structure, morphology and nature of dispersion, parameters of porous structure, and thermal as well as electrokinetic properties. The solgel process proved very effective in the synthesis of highly active powders, as evidenced by the very high values obtained for the products' surface area. It was also confirmed that the physicochemical parameters are strongly dependent on the mass ratio of the reactants and on the method of final treatment of the precipitates.