Publication date: 15th December 2025
The thermal stability of MXenes fundamentally constrains their practical implementation in next-generation electrochemical energy-storage systems. Since their discovery as two-dimensional transition-metal carbides and nitrides, ¹ MXenes have demonstrated exceptional electrical conductivity and tunable surface chemistry. However, their intrinsic thermodynamic metastability makes them susceptible to structural and chemical transformations under elevated temperatures, limiting long-term application. ²˒³ A detailed, real-time understanding of their degradation pathways and phase evolution remains essential for defining stability limits and guiding material design.
Here, we employ in-situ and operando scanning transmission electron microscopy ((S)TEM), complemented by 4D STEM analysis, to directly observe the atomic-scale thermal degradation and new phase formation processes in Ti3C2Tx MXene. This approach enables dynamic observation of structural evolution and thermal degradation behaviour of Ti3C2Tx MXene in temperature range from 25 °C to 1200 °C.
At elevated temperatures, defect accumulation facilitates atomic rearrangement within the carbide lattice, driving the formation of new phases. Diffraction and 4D STEM analysis confirm the gradual transition from a well-ordered two-dimensional framework to heterogeneous regions composed of transformed phases. This evolution progressively compromises structural coherence and leads to partial collapse of the layered architecture. Under ambient conditions operando electrochemical cycling, we observe stacking, fragmentation and irreversible degradation of the 2D morphology.
The observed transformation sequence—termination desorption, defect evolution, phase formation, oxidation, and structural collapse—provides direct atomic-scale evidence linking thermal exposure to functional degradation in MXenes. Additionally, in realistic battery environments, heat generated by resistive losses and high-rate operation can accelerate these pathways. The structural and phase changes identified here offer a mechanistic explanation for performance decay reported in MXene-based electrodes. 4
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