Despite the encouraging inherent properties of and research progress on two-dimensional (2D) MoS2, an ongoing issue associated with oxidative instability remains unsolved for practical optoelectronic applications. Thus, in-depth understanding of the oxidation behavior of large-scale and homogeneous 2D MoS2 is imperative. In this study, the structural and chemical transformations of large-area MoS2 multilayers were investigated by air-annealing at various temperatures and times by performing Raman spectroscopy, X-ray photoelectron spectroscopy, and atomic force microscopy. The results explicitly indicate the temperature- and time-dependent oxidation effects: heat-driven elimination of redundant residues, internal strain stimulated by the formation of Mo–O bonds, deterioration of the MoS2 crystallinity, layer thinning, and morphological transformation from 2D MoS2 layers into particles. Photoelectrical characterization of the air-annealed MoS2 was implemented to capture the link between the oxidation behavior of large-scale MoS2 multilayers and their photoelectrical properties.
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