Abstract: CuFe₂O₄ hollow microspheres were successfully synthesized via sol-gel two-step method with only several simple primary raw materials.The PCM and the SEM photographs showed that the as-prepared spheres were hollow and the diameters were mostly among 8-30μm.In addition,the PCM images showed that the yield and quality changed along with the blowing agent content in the raw material.XRD and EDX analyses indicated that the as-prepared spheres were mainly composed of CuFe₂O₄ and a small amount of the elementary substance Cu.Ultraviolet spectrum analysis showed that the achieved CuFe₂O₄ hollow spheres exhibited both the catalysis and the adsorption properties.