Scalable delamination of multilayer MXene via high-pressure homogenization and subsequent surface functionalization

Unlocking the full potential of MXenes for practical applications requires delamination methods that are scalable, robust, and both cost- and time-efficient for large-scale production. Equally important is ensuring that the delaminated MXene is compatible with surface functionalization strategies that enhance oxidation stability, enable tunable dispersion in diverse solvents, and allow precise control over physicochemical properties. Here we demonstrate high-pressure homogenization (HPH) as an effective, rapid, scalable method to delaminate multilayer Ti3C2Tx (Tx = -OH, -O, -F, etc.) MXene into few-layer nanosheets. Exfoliation efficiency is tuned via the number of HPH passes, leveraging combined shear, cavitation, and impact forces—eliminating chemical intercalants, washing steps, and reducing material waste. The delaminated MXenes are functionalized using two catechol-based ligands: polycatechol and catechol-grafted polyvinylpyrrolidone. Enhanced delamination improves functionalization efficiency by increasing surface accessibility. Notably, HPH-delaminated MXene shows no oxidation post-exfoliation but exhibits slight oxidation during functionalization. This work lays the foundation for optimizing scalable delamination and functionalization processes, critical for advancing MXene applications. This paper demonstrates that high-pressure homogenization is a rapid and scalable process for delaminating a multilayer MXene into few-layer nanosheets, followed by improved functionalization with catechol-based ligands due to surface accessibility.