Hydrothermal‐Assisted High‐Yield Production of Large‐Area Ti ₃ C ₂ T x MXene for High‐Performance Transparent Conductive and EMI‐Shielding Films

MXenes, a family of two‐dimensional transition metal carbides and nitrides, are promising for optoelectronic and shielding applications owing to their high electrical conductivity and tunable surface chemistry. However, their commercialization is hindered by poor oxidation stability, low‐yield synthesis, hydrofluoric acid‐based etching, and difficulty in producing large‐area flakes. Here, we report an integrated hydrothermal etching and water‐only delamination strategy for scalable production of high‐quality, large‐area MXene. Optimized hydrothermal etching enabled efficient Al removal while preserving multilayer MXene structure, providing an ideal precursor for the subsequent production of high‐quality MXene flakes. Water‐assisted delamination achieved few‐layer flakes with a reproducible yield (∼80%). The resulting flakes exhibited a large average lateral size (∼5.0 µm) and high average electrical conductivity (18 067 S cm −1 ) without size selection. Additive‐free aqueous dispersions were directly compatible with slot‐die coating, enabling uniform transparent conductive films with a high electrical‐to‐optical conductivity ratio (σ DC /σ OPT ) of 60.45. The films maintained stable electrical conductivity for over two weeks under 100% relative humidity and demonstrated an exceptional electromagnetic interference‐specific shielding effectiveness per thickness of 1.484 × 10 6 dB·cm 2 ·g −1 . This work establishes a safe and industry‐compatible pathway for producing high‐performance MXene transparent electrodes and multifunctional shielding materials, advancing the practical commercialization of MXene‐based technologies.