Monodisperse CoFe2O4and Co0.4Zn0.6Fe2O4hollow nanospheres were synthesized in large scale by solvothermal method in ethylene glycol solution. The structure, shape and size of the samples were investigated by Fourier Transform infrared, X-ray powder diffraction and scanning electron microscopy. The results indicate that the products are spherical with an average diameter less than 200 nm. Magnetic studies revealed that the saturation magnetization of Co0.4Zn0.6Fe2O4is 78.6 emu/g, higher than the CoFe2O4, which is 69 emu/g, while the coercivity of the Co0.4Zn0.6Fe2O4is 184 Oe , obviously lower than that of CoFe2O4which is 832 Oe. The electromagnetic parameters were measured at 2-18 GHz using HP8722ES vector network analyzer and then the microwave absorption properties were calculated through the transmission line theory. As to the Co0.4Zn0.6Fe2O4, the absorption bandwidth with reflection loss below-10 dB is up to 3GHz, from 10GHz to 13GHz with a thickness of 2 mm. A maximum reflection loss-45.6 dB was found at 12.9 GHz for the CoFe2O4with a thickness of 1.8 mm. As a result, the as-prepared hollow nanospheres show good prospects of being applied in EM wave absorption materials.