The interface produced by vapor deposition of Mn on the MoS2(0001) surface has been studied insitu by high‐resolution photoelectron spectroscopy using synchrotron radiation. The evolution of the Mo 3d, Mn 3p, and S 2p core levels and of the valence‐band spectra during growth of thin films (10–58 Å) is consistent with partial conversion of the Mn overlayer to MnS via the overall reaction 2Mn+MoS2→2MnS+Mo. The persistence of the substrate components of the Mo 3d and S 2p spectra for thicknesses >35 Å are consistent with the Volmer–Weber growth mode. Annealing a 58‐Å film to 770 K resulted in an overlayer film consisting mostly of MnS coexisting with some metallic Mn. Analysis of the Mo 3d core levels indicates the production of a MoS2(0001) surface with S vacancy defects. Annealing to temperatures between 850 and 1040 K drove the reaction to completion (as shown by the valence band and Mn 3p core level spectra). Annealing of the sample to 1130 K resulted in uncovering the MoS2(0001) surface due to breakup of the reacted layer. In addition, low‐energy electron diffraction indicated the formation of (0001)–2×2 regions on the surface. This surface structure is interpreted in terms of an ordered, MoS2−x sulfur vacancy defect structure rather than a Mn–Mo–S compound.

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