EMW radiation will interfere with the normal operation of digital equipment and electronic components, and it is difficult to guarantee people's information security. [4,5] More seriously, studies have shown that EMW can interfere with the inherent magnetic field of the human body, increasing the risk of skin diseases, heart disease, cancer, and other diseases, and pose a great threat to health. [6][7][8][9] Therefore, it is urgent to develop advanced and efficient absorbing materials. [10] The absorption behavior of high-performance EMW absorbing materials depends heavily on the electromagnetic parameters and impedance-matching properties. [11,12] In turn, they are closely related to the size, microstructure, composition, and geometry of the material. [13][14][15] However, in addition to the inherent magnetic and dielectric properties, the material itself will affect the impedance-matching characteristics of the material. In order to improve the electromagnetic absorption property, the reasonable design and construction of absorbing materials with special microstructure are also very important for the attenuation of EMW. It is generally believed that the properties of materials are highly related to the nanostructures of materials. [16] Therefore, researchers have made great efforts to design and regulate materials with special structures. such as arranged structures, porous structures, hollow structures, and core-shell structures, in which especially hollow and porous structures with low density and large hollow interfaces have aroused the interest of researchers. [17][18][19] In absorbing materials, the design of voids or shells can efficiently decrease the density of materials for lightweight purposes, and the impedancematching characteristics can be adjusted by reducing the complex permittivity. The existence of this internal void also gives it multiple reflections and scattering effects, which is conducive to prolonging the propagation path of EMWs to enhance attenuation. [20][21][22] As a typical class of dielectric loss materials, carbides have been highly sought after by researchers because of their various remarkable advantages such as good thermal stability, high mechanical strength, and high resistance to oxidation and corrosion. [23][24][25][26][27][28][29] Especially in the field of EMW absorption, researchers have used the semiconducting nature of carbide to regulate the dielectric constant of carbon materials by compounding with carbon materials to effectively regulate the In order to achieve excellent electromagnetic wave (EMW) absorption properties, the microstructure design and component control of the absorber are critical. In this study, three different structures made of Mo 2 C/C hollow spheres are prepared and their microwave absorption behavior is investigated. The Mo 2 C/C double-shell hollow spheres consisting of an outer thin shell and an inner rough thick shell with multiple EMW loss mechanisms exhibit good microwave absorption properties. In order to further improve the microwave abso...