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Abstract Janus structures have unique properties due to their distinct functionalities on opposing faces, but have yet to be realized with flowing liquids. We demonstrate such Janus liquids with a customizable distribution of nanoparticles (NPs) throughout their structures by joining two aqueous streams of NP dispersions in an apolar liquid. Using this anisotropic integration platform, different magnetic, conductive, or non-responsive NPs can be spatially confined to opposite sides of the original interface using magnetic graphene oxide (mGO)/GO, Ti₃C₂T_x/GO, or GO suspensions. The resultant Janus liquids can be used as templates for versatile, responsive, and mechanically robust aerogels suitable for piezoresistive sensing, human motion monitoring, and electromagnetic interference (EMI) shielding with a tuned absorption mechanism. The EMI shields outperform their current counterparts in terms of wave absorption, i.e., SE_T ≈ 51 dB, SE_R ≈ 0.4 dB, and A = 0.91, due to their high porosity ranging from micro- to macro-scales along with non-interfering magnetic and conductive networks imparted by the Janus architecture. 

Abstract MXene and graphene cryogels have demonstrated excellent electromagnetic interference (EMI) shielding effectiveness due to their exceptional electrical conductivity, low density, and ability to dissipate electromagnetic waves through numerous internal interfaces. However, their synthesis demands costly reduction techniques and/or pre‐processing methods such as freeze‐casting to achieve high EMI shielding and mechanical performance. Furthermore, limited research has been conducted on optimizing the cryogel microstructures and porosity to enhance EMI shielding effectiveness while reducing materials consumption. Herein, a novel approach to produce ultra‐lightweight cryogels composed of Ti₃C₂T_x/graphene oxide (GO) displaying multiscale porosity is presented to enable high‐performance EMI shielding. This method uses controllable templating through the interfacial assembly of filamentous‐structured liquids that are readily converted into EMI cryogels. The obtained ultra‐flyweight cryogels (3–7 mg cm⁻³) exhibit outstanding specific EMI shielding effectiveness (33 000–50 000 dB cm² g⁻¹) while eliminating the need for chemical or thermal reduction. Furthermore, exceptional shielding is achieved when the Ti₃C₂T_x/GO cryogels are used as the backbone of conductive epoxy nanocomposites, yielding EMI shielding effectiveness of 31.7–51.4 dB at a low filler loading (0.3–0.7 wt%). Overall, a one‐of‐a‐kind EMI shielding system is introduced that is readily processed while affording scalability and performance.