Anjali Sugunan, Anusree V. Rethnakumaran, Athul Beena Radhakrishnan, Mini Mol Menamparambath
A simple liquid/liquid interfacial in situ polymerization strategy is employed to engineer MXene-based nanohybrids through controlled interlayer expansion and hybridization. The approach exploits spatially confined in situ polymerization of pyrrole at the chloroform/water interface, where pyrrole molecules adsorb onto Ti 3 C 2 T x surfaces and partially access interlayer regions, followed by controlled polymer growth. This process induces polymer-assisted structural expansion, improves MXene dispersion, and promotes the formation of an intimate MXene/PPy interface. Subsequent incorporation of copper into the preorganized MXene/PPy framework yields a ternary MXene/PPy/Cu nanohybrid with enhanced active site accessibility and improved charge transport characteristics. The nanohybrid-modified carbon yarn electrode exhibits a pronounced electrochemical response toward uric acid (UA), highlighting the synergistic contributions of conductive PPy, catalytic Cu, and structurally engineered MXene, delivering a linear detection range of 1–30 μM and a detection limit of 0.5 μM. This detection limit is comparable to or better than many recently reported MXene-based and other electrochemical UA sensors, highlighting the benefit of the integrated MXene/PPy/Cu architecture. The sensor demonstrates good selectivity in the presence of common interferents, along with reliable repeatability and reproducibility and consistent performance in spiked human serum and urine samples, with recoveries of 90–110%. This work introduces a simple yet effective interfacial strategy to engineer MXene-based nanohybrids with synergistic combination of a conductive MXene/polymer network and catalytically active metal sites for advanced electrochemical sensing applications.