Coprecipitation and hydrothermal method were utilized for the synthesis of Co‐doped Ni‐Zn ferrite and barium titanate nanoparticles. The microwave absorption properties of Co‐doped Ni‐Zn ferrite/barium titanate nanocomposites with single layer structure were studied in the frequency range of 8.2–12.4 GHz.The spectroscopic characterizations of the nanocomposites were examined using X‐ ray diffraction, scanning electron microscopy, transmission electron microscopy and dynamic light scattering measurement. Thermogravimetric analysis indicated the high thermal stabilities of the composites. The composite materials showed brilliant microwave absorbing properties in a wide range of frequency in the X‐band region with the minimum return loss of −42.53 dB at 11.81 GHz when sample thickness was 2 mm and the mechanisms of microwave absorption are happening mainly due to the dielectric loss. Compared with pure Co‐doped Ni‐Zn ferrite, Co‐doped Ni‐Zn ferrite/BaTiO3 composites exhibited enhanced absorbing properties. The microwave absorbing properties can be modulated by controlling the BaTiO3 content of the absorbers and also by changing the sample thicknesses. Therefore, these composites can be used as lightweight and highly effective microwave absorbers. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014, 131, 39926.