AbstractThe development of high‐temperature electromagnetic (EM) wave absorbing materials is an important direction for achieving radar stealth in high‐speed aircraft. In this study, HfC–SiCf composite ceramics with 3D reticular structure were synthesized in one‐step using the molten‐salt‐assisted carbon thermal reduction method. During the synthesis process, SiC grew in situ into a fibrous structure with a diameter of 500 nm and lengths ranging from 2 to 30 µm. By adjusting the molar ratio of HfC to SiC, the HfC‐30 mol% SiC (HS30) exhibited the best EM absorption performance at room temperature, with a minimum reflection loss (RLmin) of −31.4 dB at 16.1 GHz and an effective absorption bandwidth (EAB) of 4.6 GHz. The excellent absorption performance was attributed to the 3D reticular structure composed of SiC fibers, HfC bulk, and HfC nanoparticles, which significantly increased the number of pores and heterogeneous interfaces in the material. These microinterfaces induced interface polarization effects, thereby effectively enhancing the EM absorption. As the temperature increased, the EM absorption performance declined. At 900°C, the HS30 sample exhibited an EAB of 1.18 GHz from 12.4 to 13.58 GHz and an RLmin of 22.6 dB at 13.0 GHz. This research provides references for understanding the effects of material composition and structure on EM absorption performance.