High Quality MoS ₂ Layered Thin Films Obtained by Ionized Jet Deposition Investigated by X‐ray Absorption Spectroscopy at S L _2,3 and Mo M _2,3 Edges

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.