Comparative Effects of Hydrazine and Thermal Reduction Methods on Electromagnetic Interference Shielding Characteristics in Foamed Titanium Carbonitride MXene Films

The urgent need for the development of micro‐thin shields against electromagnetic interference (EMI) has sparked interest in MXene materials owing to their metallic electrical conductivity and ease of film processing. Meanwhile, postprocessing treatments can potentially exert profound impacts on their shielding effectiveness (SE). This work comprehensively compares two reduction methods, hydrazine versus thermal, to fabricate foamed titanium carbonitride (Ti3CNTx) MXene films for efficient EMI shielding. Upon treatment of ≈ 100 µm‐thick MXene films, gaseous transformations of oxygen‐containing surface groups induce highly porous structures (up to ≈ 74.0% porosity). The controlled application of hydrazine and heat allows precise regulation of the reduction processes, enabling tailored control over the morphology, thickness, chemistry, and electrical properties of the MXene films. Accordingly, the EMI SE values are theoretically and experimentally determined. The treated MXene films exhibit significantly enhanced SE values compared to the pristine MXene film (≈ 52.2 dB), with ≈ 38% and ≈ 83% maximum improvements for the hydrazine and heat‐treated samples, respectively. Particularly, heat treatment is more effective in terms of this enhancement such that an SE of 118.4 dB is achieved at 14.3 GHz, unprecedented for synthetic materials. Overall, the findings of this work hold significant practical implications for advancing high‐performance, non‐metallic EMI shielding materials. Hydrazine and heat postprocessing treatments of titanium carbonitride MXene films trigger the formation of highly porous structures through efficient reduction of oxygenated surface terminations releasing gaseous products. Extensive evaluation of microstructural, chemical, electrical, and shielding parameters endows both processes with meticulous customizability to secure the utmost EMI shielding performance, with heat treatment showing superior results.