Abstract2D transition metal dichalcogenide materials have attracted increasing attention as active surface‐enhanced Raman spectroscopy (SERS) platforms. In this study, the influence of n‐ and p‐type doping of exfoliated MoS2 (exMoS2) hybrids on the SERS performance is investigated, employing Rhodamine 6G (R6G) as a probe molecule. It is demonstrated that n‐doped exMoS2 hybrids (exMoS2 mixed with C60, graphene, and sodium dodecyl sulfate) exhibit enhanced SERS intensities, while p‐doping (exMoS2 mixed with TCNQ) resulted in inhibited SERS enhancement. A key discovery is the linear relationship between Raman enhancement of MoS2/dopant hybrids and the difference in their LUMO energy levels, which dictate the degree and direction of charge transfer. Interestingly, MC60‐4, a C60‐doped hybrid, deviates from the linear relationship, displaying remarkable SERS enhancement owing to its chemical interaction and unique Raman scattering activity. The findings provide critical insights into the SERS enhancement behavior of doped MoS2, facilitating precise tuning of SERS intensities by manipulating the MoS2 doping state.
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