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MXenes are promising supports for anchoring metal single atoms due to their versatile composition, well-defined nanostructures, and suitable conductivity. However, metal single atoms are usually coordinated with surface terminal groups (-O, -OH, -Cl, etc.) of MXenes via conventional wet-impregnation, resulting in limited electronic structure modification. Through a NiCl2 molten salt etching method, we observed that Ni single atoms could be in-situ doped in the lattice of MXenes analogue TiC0.5N0.5 support (denoted as Ni1/TiC0.5N0.5), resulting in much larger charge transfer from Ni atoms to adjacent Ti atoms, and thus increasing the electronic density of these Ti atoms. When used for NO2 sensing, Ni1/TiC0.5N0.5 exhibited excellent response sensitivity (ultra-low limit of detection ∼ 10 ppb), selectivity, and good stability at room temperature. This study provides an effective strategy for producing MXenes analogue supported metal single atoms for potential application in gas sensing. [ABSTRACT FROM AUTHOR]