Sol-gel derived nano-composites silica-gel doped with different iron oxide concentrations at (3.5, 11, 33 and 37 mol. %) sintered at constant temperature at 1170^°C, are illustrated in this work. Structure, surface morphology, high frequency dielectric and magnetic trends of the mentioned nano-composites analyzed and investigated through XRD, UV-Vis, TEM, FESEM and Magnetic hysteresis curves. Raman micro-spectroscopy gives rise to samples homogenous distribution. XRD illustrate that the Hematite (α-Fe₂O₃) is the optimum phase rather than the Maghemite (γ-Fe₂O₃) and Magnetite (Ԑ- Fe₂O₃). Big amount of Hematite (α-Fe₂O₃) crystalline nano-particles are expected at 37 mol. % of Fe₂­O₃. XRD confirmed that the average crystallite size increased from (25-31) nm with increasing the concentration of (α-Fe₂O₃) from 3.5 up to 37 mol%. The A.C. conductivity σ_ac increased by increasing the α-Fe₂O₃ content, according to the presence of oxygen vacancy and the crystalline size increases. The decreasing behavior in magnetization value (M_s) is related to the changes of the crystallite size, magnetic iron oxide particles and concentration. All analysis explains Hematite is extremely stable at ambient conditions and at high temperatures, so it is the better for particular applications.