In order to prevent the microwave leakage and mutual interference, more and more microwave absorbing devices are added into the design of electronic products to ensure its routine operation. In this work, we have successfully prepared MoS2/TiO2/Ti3C2Tx hierarchical composites by one-pot hydrothermal method and focused on the relationship between structures and electromagnetic absorbing properties. Supported by comprehensive characterizations, MoS2 nanosheets were proved to be anchored on the surface and interlayer of Ti3C2Tx through a hydrothermal process. Additionally, TiO2 nanoparticles were obtained in situ. Due to these hierarchical structures, the MoS2/TiO2/Ti3C2Tx composites showed greatly enhanced microwave absorbing performance. The MoS2/TiO2/Ti3C2Tx composites exhibit a maximum reflection loss value of −33.5 dB at 10.24 GHz and the effective absorption bandwidth covers 3.1 GHz (13.9–17 GHz) at the thickness of 1.0 mm, implying the features of wide frequency and light weight. This work in the hierarchical structure of MoS2/TiO2/Ti3C2Tx composites opens a promising door to the exploration of constructing extraordinary electromagnetic wave absorbents.

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The fabrication of ultra‐high performance absorbers with low thickness, light weight, hierarchical structure, and strong microwave absorption (MA) capability in a wide frequency range is a critical objective of the scientific community. The unique two‐dimensional lamellar and sandwich‐like structure of MoS2 (S‐Mo‐S) in combination with Ti3C2Tx offers exceptional metallic features, an enriched surface area and a hierarchical structure; hence, it is an appealing alternative to high‐efficiency microwave absorbers. Herein, two‐dimensional C/MoS2‐functionalized Ti3C2Tx hierarchical structures with superior attenuation capabilities (dielectric losses) are creatively designed and fabricated, and a minimal reflection loss (RLmin) of −42.7 dB is achieved at a thickness of only 1.5 mm. These excellent microwave absorption properties are attributed to better impedance matching, which is due to the tunable complex permittivity; intensive interfacial polarization, which stems from the numerous interfaces of multiple components; multiple scattering, which originates from the presence of plentiful two‐dimensional nanosheets; and ohmic loss, which arises from the formation of conductivity networks. The interconnected sandwich‐like and layered structure is proven to be an effective strategy for enriched microwave absorption by functionalized Ti3C2Tx nanocomposites.