Ti ₃ C ₂ T <i> _x </i> MXene as an Active Template for Accelerated Assembly and Structuring of Electroactive Ce‐MnO ₂ /PEDOT Nanohybrids at Bisolvent Interface

ABSTRACT MXenes, a cutting‐edge family of two‐dimensional transition metal carbides and nitrides, distinguish themselves through an exceptional synergy of metallic conductivity, tunable surface chemistry, and structural versatility, placing them at the forefront of advanced materials research. While extensively studied for energy storage, catalysis, and sensing, their potential in interfacial polymerization for the in situ generation of polymer/nanomaterial hybrids remains largely untapped. In this study, Ti 3 C 2 T x MXene is employed as a conductive and reactive interface to facilitate the in situ generation of Ce‐doped MnO 2 /PEDOT (CMP) nanohybrid through a liquid/liquid (L/L) interface‐assisted oxidative polymerization strategy, yielding a MXene‐based Ce‐doped MnO 2 /PEDOT nanohybrid (MCMP3). Beyond serving as a structural scaffold, the MXene surface accelerates polymerization, promoting rapid hybrid formation and enabling one‐step integration of the conducting polymer and doped metal oxide within a unified architecture. As a result of this MXene‐assisted interfacial process, the polymerization proceeds significantly faster, reducing the reaction time from 24 to 4 h under ambient conditions. The PXRD, UV–vis, and Raman analyses confirmed the compositional optimization of Ce‐doping with the characteristic features of layered K‐birnessite‐type MnO 2 . TEM and XPS analyses of the MCMP3 further confirmed its morphology, elemental composition, and successful nanohybrid formation. Pendant drop tensiometry substantiated the MXene‐assisted acceleration of polymerization, demonstrating that MXene facilitates rapid polymer growth and interfacial anchoring of amphiphilic intermediates, thereby governing the controlled assembly of MCMP3 at the L/L interface. DFT calculations further elucidated sulfur‐mediated chemisorption of EDOT onto Ti active sites of the MXene. These physicochemical characteristics are reflected in the electrochemical response of the MCMP3 nanohybrid, which exhibited a detection limit of 59.7 nM toward metronidazole (MDZ), a widely used nitroimidazole antibiotic. This performance confirms the effective electrochemical activity of the hybrid system and supports its potential applicability for MDZ sensing. Additionally, real‐time analysis of both milk and native lake water substantiates its viability for pharmaceutical and environmental applications. These findings establish MXene as an exceptional facilitator for the in situ generation of multifunctional polymer/nanomaterial architectures, opening avenues for the design and development of next‐generation electrochemical devices.