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Control of surface functionalization of MXenes holds great potential, and inparticular, may lead to tuning of magnetic and electronic order in the recentlyreported magnetic Cr2TiC2Tx. Here, vacuum annealing experiments of Cr2TiC2Txare reported with in situ electron energy loss spectroscopy and novel in situCr K-edge extended energy loss fine structure analysis, which directly tracksthe evolution of the MXene surface coordination environment. These in situprobes are accompanied by benchmarking synchrotron X-ray absorption finestructure measurements and density functional theory calculations. With theetching method used here, the MXene has an initial termination chemistry ofCr2TiC2O1.3F0.8. Annealing to 600 C results in the complete loss of -F, but -Otermination is thermally stable up to (at least) 700 C. These findingsdemonstrate thermal control of -F termination in Cr2TiC2Tx and offer a firststep towards termination engineering this MXene for magnetic applications.Moreover, this work demonstrates high energy electron spectroscopy as apowerful approach for surface characterization in 2D materials.

Multi-modal Spectroscopic Study of Surface Termination Evolution in Cr2TiC2Tx MXene