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Nanoparticles with aerodynamic diameters of less than 100 nm pose serious problems to human health due to their small size and large surface area. Despite continuous progress in materials science to develop air remediation technologies, efficient nanoparticle filtration has appeared to be challenging. This study showcases the great promise of MXene-coated polyester textiles to efficiently filter nanoparticles, achieving a high efficiency of ~90% within the 15–30 nm range. Using alkaline earth metal ions to assist textile coating drastically improves the filter performance by ca. 25%, with the structure–property relationship thoroughly assessed by electron microscopy and X-ray computed tomography. Such techniques confirm metal ions’ crucial role in obtaining fully coated and impregnated textiles, which increases tortuosity and structural features that boost the ultimate filtration efficiency. Our work provides a novel perspective on using MXene textiles for nanoparticle filtration, presenting a viable alternative to produce high-performance air filters for real-world applications. 

Abstract MXenes are a class of 2D materials that have gained significant attention for their potential applications in energy storage, electromagnetic interference shielding, biomedicine, and (opto)electronics. Despite their broad range of applications, a detailed understanding of the internal architecture of MXene‐based materials remains limited due to the lack of effective 3D imaging techniques. This work demonstrates the application of X‐ray micro‐computed tomography (micro‐CT) to investigate various MXene systems, including nanocomposites, coated textiles, and aerogels. Micro‐CT enables high‐resolution, 3D visualization of the internal microstructure, MXene distribution, infiltration patterns, and defect formations, which significantly influence the material's performance. Moreover, the typical technical challenges and limitations encountered during sample preparation, scanning, and post‐processing of micro‐CT data are discussed. The information obtained from optical and electron microscopy is also compared with micro‐CT, highlighting the unique advantages of micro‐CT in providing comprehensive 3D imaging and quantitative data. This study highlights micro‐CT as a powerful and nondestructive imaging tool for characterizing MXene‐based materials, providing insights into material optimization and guidelines for developing future advanced applications.