Synthesis and Evaluation of Molybdenum Imido-Thiolato Complexes for the Aerosol-Assisted Chemical Vapor Deposition of Nitrogen-Doped Molybdenum Disulfide
Nathan C. Ou, Konstantin Preradovic, Erik T. Ferenczy, Courtney B. Sparrow, Ian M. Germaine, Titel Jurca, V. Crăciun, Lisa McElwee‐White
Abstract
Molybdenum bis(imido) bis(thiolato) complexes of the type Mo(NtBu)2(SR)2 (R = tBu (1), iPr (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(NtBu)2(StBu)2 to that of pristine MoS2 grown from Mo(StBu)4 were carried out. The material was characterized as MoS2 with nitrogen doping by the presence of the 2H-MoS2 1E2g and A1g 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.