Abstract: Based on the technique of micro fluid injection molding, RF hollow microspheres were synthesized by using dibutyl phthalate as oil phase, RF solution as water phase, and by sol-gel, solvent exchanging and supercritical drying. The components, morphology, aperture, and diameter distribution of RF hollow microspheres were characterized by infrared spectrum, X-ray micro analysis, TEM, and nitrogen adsorption-desorption respectively.The results show that RF hollow microsphere is monolayered and has a typical structure of the porous aerogel. The pores are consisting of nearly uniform nano-particles about 10 nm in diameter, and their average aperture is about 20 nm. The sphericity and concentricity of the monolayer hollow microsphere is higher than 95%, the diameter distribution of RF hollow mic