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Abstract Ultrathin 2D metal oxides are a high‐performance class of transparent conducting materials capable of overcoming the traditional limitations of inorganic flexible electronics. The low temperature, thermodynamically favorable synthesis of 2D oxides at liquid metal interfaces offers the potential for printing these materials over large areas at unprecedented speeds with sub‐nanometer scale precision. However, these native oxides are sub‐stoichiometric and highly conductive, so new strategies are needed that can precisely engineer the electrostatics and enhance stability. In this work, the crystalline vs. amorphous phase of 2D oxides is engineered via alloying of ternary In_1‐ySn_yO_xand ultralow deposition temperatures (120–160 °C) are afforded by In‐Sn eutectics. This approach is extended to rapid assembly of nanoscale (3–5 nm per layer) vertical 2D homojunctions with electrostatically favorable grading from high density of states front channels to lower density of states back‐channels. Detailed materials characterization reveals how this platform enhances electron mobility while improving resilience under bias‐stress in metal oxide transistors. Devices based on amorphous 2D oxide homojunctions with high‐k sol‐gel ZrO_xdielectrics achieve excellent electron mobility (30 cm²/V·s), steep switching (SS of 100 mV dec⁻¹), I_on/offof 10⁷and 10X reduced bias‐stress shifts, presenting an ideal strategy for high‐performance flexible oxide electronics. 

Abstract 3D continuous mesoscale architectures of nanomaterials possess the potential to revolutionize real‐time electrochemical biosensing through higher active site density and improved accessibility for cell proliferation. Herein, 3D microporous Ti₃C₂T_XMXene biosensors are fabricated to monitor antibiotic release in tissue engineering scaffolds. The Ti₃C₂T_X‐coated 3D electrodes are prepared by conformal MXene deposition on 3D‐printed polymer microlattices. The Ti₃C₂T_XMXene coating facilitates direct electron transfer, leading to the efficient detection of common antibiotics such as gentamicin and vancomycin. The 3D microporous architecture exposes greater electrochemically active MXene surface area, resulting in remarkable sensitivity for detecting gentamicin (10–1 mM) and vancomycin (100–1 mM), 1000 times more sensitive than control electrodes composed of 2D planar films of Ti₃C₂T_XMXene. To characterize the suitability of 3D microporous Ti₃C₂T_XMXene sensors for monitoring drug elution in bone tissue regeneration applications, osteoblast‐like (MG‐63) cells are seeded on the 3D MXene microlattices for 3, 5, and 7 days. Cell proliferation on the 3D microporous MXene is tracked over 7 days, demonstrating its promising biocompatibility and its clinical translation potential. Thus, 3D microporous Ti₃C₂T_XMXene can provide a platform for mediator‐free biosensing, enabling new applications for in vivo monitoring of drug elution.