Magnetic materials are one of the promising material for their special magnetic properties and other functionalities. A sol-gel process in reverse microemulsion combined with solvent-thermal technique(ME-SG-ST) was developed for synthesizing nano-sized mesoporous SiO2/CoFe2O4(SCF). Fourier transform infrared spectrometry, TG-DSC, X-ray diffraction, TEM, BET specific surface area measurement, N2 adsorption-desorption and magnetic analysis were used to characterize the structure and magnetism property. Results showed that spinel CoFe2O4 was uniformly dispersed in nanosized SCF particles. The prepared SCF particles possessed mesopore structure and excellent paramagnetism, and will become great promising materials as the supports of catalyst and absorbents for biological and drugs.