In this work, double-loss Ti3SiC2/Co3Fe7 powders were synthesized by carbothermic reduction method. X-ray diffraction (XRD) confirmed the successful synthesis of the Ti3SiC2/Co3Fe7 powders, and scanning electron microscope (SEM) images showed the Co3Fe7 particles uniformly scattering on the surface of Ti3SiC2. Microwave absorption properties of the Ti3SiC2/Co3Fe7 powders were investigated in the frequency range from 8.2 to 12.4GHz (X-band). The high dielectric and magnetic loss give rise to a favorable microwave absorption performance. The sample with a thickness of 2.4mm owns an effective absorption bandwidth (reflection loss below − 10dB) of 8.8–11.9GHz, with a minimum value of − 31.2dB at 10.0GHz. This study is an important exploration of microwave absorption materials for high temperature application.