ABSTRACT We present a comparative soft x‐ray absorption spectroscopy (XAS) study of the sulfur L 2 , 3 and molybdenum M 2 , 3 absorption edges in MoS 2 prepared by different fabrication routes, including bulk crystallization, mechanical exfoliation, chemical vapor deposition (CVD), and ionized jet deposition (IJD). The S L 2 , 3 edges reveal pronounced differences in pre‐edge and main‐edge fine structure that sensitively reflect the degree of structural order, dimensionality, and electronic hybridization between S 3p and Mo 4d states. Bulk, exfoliated, and CVD‐grown samples exhibit well‐resolved multiple features characteristic of layered and ordered two‐dimensional (2D) MoS 2 , whereas as‐deposited IJD‐grown films display broadened, weakly structured spectra consistent with an amorphous phase and poorly defined stoichiometry. Upon moderate annealing at 250°C, IJD‐grown films develop clear spectral signatures of layered MoS 2 , indicating the formation of an ordered crystalline 2H‐MoS 2 phase. Complementary analysis of the Mo M 2 , 3 edges shows a concomitant narrowing and energy shift of the M 3 feature toward values typical of well‐ordered 2D MoS 2 . These results demonstrate that S L 2 , 3 and Mo M 2 , 3 XAS provide a sensitive probe of synthesis‐dependent electronic structure in MoS 2 and confirm IJD as a viable, low‐temperature route to electronically ordered 2D MoS 2 phases.
Giovanelli et al. (Mon,) studied this question.