The method for template hydrothermal synthesis (HTS method) with use of various precursors of iron oxide, namely with iron sulfate and iron chloride salts mixed at ratios of 1:1 and 1:2, iron nitrate, goethite, and γ-Fe203 stabilized with oleic acid, was applied to synthesize iron-silica composites containing [Fe] and [Si] components at ratios of 0.025-0.2. To prepare mesoporous Fe2O3-SiO2 systems featured by high proportions of the iron-oxide component (up to [Fe] [Si] = 1) and by high values of specific surface area during the THS process, a “fractional precipitation” method was proposed. Textural-structural characteristics of the obtained materials were comparatively appraised.