Synthesis and Evaluation of Molybdenum Imido-Thiolato Complexes for the Aerosol-Assisted Chemical Vapor Deposition of Nitrogen-Doped Molybdenum Disulfide

摘要

Molybdenum bis(imido) bis(thiolato) complexes of the type Mo((NBu)-Bu-t)(2) (SR)(2) (R = Bu-t (1), Pr-i (2)) were synthesized and evaluated as precursors for the aerosol-assisted chemical vapor deposition (AACVD) of nitrogen-doped molybdenum disulfide. Decomposition of the precursors was examined using mass spectrometry and thermolysis experiments, and the predominant pathways were those that involved proton transfer from a methyl group on a thiolato ligand. Thermal behavior, volatility, and enthalpies of sublimation were analyzed using TGA. Comparative studies of the nitrogen-doped MoS2(N-MoS2) grown from Mo((NBu)-Bu-t)(2)((SBu)-Bu-t)(2) to that of pristine MoS2 grown from Mo((SBu)-Bu-t)(4) were carried out. The material was characterized as MoS2 with nitrogen doping by the presence of the 2H-MoS2 E-1(2g) and A(1g) Raman vibrational modes. The GIXRD diffraction patterns of the N-MoS2 samples were indexed to 2H-MoS2, and evidence of nitrogen doping was confirmed with the presence of Mo-N bonding by XPS and with EDS mapping. The N-MoS2 deposits displayed a nanosphere morphology which contrasted with vertical nanosheets for undoped MoS2.