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Synthesis and Evaluation of Molybdenum Imido-Thiolato Complexes for the Aerosol-Assisted Chemical Vapor Deposition of Nitrogen-Doped Molybdenum Disulfide
Organometallics ( IF 2.8 ) Pub Date : 2020-02-17 , DOI: 10.1021/acs.organomet.9b00705
Nathan C. Ou 1 , Konstantin Preradovic 2 , Erik T. Ferenczy 1 , Courtney B. Sparrow 1 , Ian M. Germaine 1 , Titel Jurca 2 , Valentin Craciun 3, 4 , Lisa McElwee-White 1
Affiliation  

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-MoS21E2g 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.

中文翻译:

氮掺杂二硫化钼的气溶胶辅助化学气相沉积钼亚氨基-硫杂钼配合物的合成与评价

合成了Mo(N t Bu)2(SR)2(R = t Bu(1),i Pr(2))类型的钼双(亚氨基)双(硫醇根)络合物,并作为气溶胶辅助的前体进行了评估氮掺杂的二硫化钼的化学气相沉积(AACVD)。使用质谱和热解实验检查了前体的分解,主要途径是那些涉及从硫醇基配体上的甲基进行质子转移的途径。使用TGA分析热行为,挥发性和升华焓。从Mo(N)生长的氮掺杂MoS 2(N-MoS 2)的比较研究相对于由Mo(S t Bu) 4生长的原始MoS 2进行了t Bu) 2(S t Bu) 2的处理。该材料被表征为的MoS 2由2H-MOS的存在下用氮掺杂2种1 Ë 2克和A 1克拉曼振动模式。将N-MoS 2样品的GIXRD衍射图样标为2H-MoS 2,并通过XPS的Mo–N键结合和EDS作图证实了氮掺杂的证据。N-MoS 2沉积物显示出纳米球形态,与未掺杂MoS 2的垂直纳米片形成对比。
更新日期:2020-02-17
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