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Synchrotron X-ray Probes of Transition-Metal Carbides/Nitrides: From Structure Tuning to In-Situ Synthesis Control
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DOI：10.1021/accountsmr.5c00351.png)
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Abstract
En 中文
ConspectusTwo-dimensional (2D) transition-metal carbides and nitrides, collectively known as MXenes, have emerged as a highly promising class of layered materials owing to their tunable physicochemical properties and broad applicability in electrochemical energy storage. However, their practical deployment is still limited by structural instability and the difficulty of achieving precise structural control, both of which stem from complex and insufficiently understood phase-evolution pathways during synthesis and operation. In this Account, we present a review on recent progress in MXenes structural engineering and synthesis regulation, emphasizing the important role of synchrotron X-ray techniques in revealing structure–property relationships and phase-evolution mechanisms. We first summarize key postetching structural regulation strategies, including intercalation, surface termination engineering, and atomic-scale configuration control. Synchrotron-based X-ray characterization enables quantitative identification of structural features that are difficult to probe by conventional methods, including the local coordination environments of intercalants and the spatial distributions of surface terminations and defects. Meanwhile, advances in in situ and operando synchrotron techniques allow direct observation of microstructural evolution under realistic operating conditions. These studies demonstrate that structural regulation strongly influences ion transport, redox behavior, and mechanical stability, thereby governing MXenes performance in diverse electrochemical energy-storage systems. We further discuss an emerging paradigm shift in the field: from postsynthetic structural tuning to active control of structural evolution during synthesis. This shift offers a more deterministic pathway toward MXenes with controlled microstructures and improved quality. In particular, synchrotron-based operando studies enable real-time monitoring of the top-down etching of MAX phases, making it possible to capture the formation of MXenes frameworks, identify transient intermediates, and elucidate the evolution of surface terminations and defects─information that is difficult to obtain using conventional ex situ methods. Finally, we highlight future opportunities in MXenes research. A deeper understanding of MXenes microstructures, their dynamic evolution, and the associated synthesis mechanisms will provide the foundation for controllable synthesis, precise structural regulation, and the scalable production of high-performance MXenes.
Keywords:
Etching
Inorganic carbon compounds
Intercalation
Layered materials
Two dimensional materials
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