二硫代羧酸钼(IV)作为用于化学气相沉积法制备二硫化钼薄膜的单源前驱体。

Molybdenum(IV) dithiocarboxylates as single-source precursors for AACVD of MoS thin films.

作者信息

Muhammad Saleh, Ferenczy Erik T, Germaine Ian M, Wagner J Tyler, Jan Muhammad T, McElwee-White Lisa

机构信息

Department of Chemistry, University of Florida, Gainesville, FL 32611-7200, USA.

Department of Chemistry, Islamia College Peshawar, 25120 Peshawar, Pakistan.

出版信息

Dalton Trans. 2022 Aug 23;51(33):12540-12548. doi: 10.1039/d2dt01852g.

Tetrakis(dithiocarboxylato)molybdenum(IV) complexes of the type Mo(SCR) (R = Me, Et, Pr, Ph) were synthesized, characterized, and prescreened as precursors for aerosol assisted chemical vapor deposition (AACVD) of MoS thin films. The thermal behavior of the complexes as determined by TGA and GC-MS was appropriate for AACVD, although the complexes were not sufficiently volatile for conventional CVD bubbler systems. Thin films of MoS were grown by AACVD at 500 °C from solutions of Mo(SCMe) in toluene. The films were characterized by GIXRD diffraction patterns which correspond to a 2H-MoS structure in the deposited film. Mo-S bonding in 2H-MoS was further confirmed by XPS and EDS. The film morphology, vertically oriented structure, and thickness (2.54 μm) were evaluated by FE-SEM. The Raman E and A vibrational modes of crystalline 2H-MoS were observed. These results demonstrate the use of dithiocarboxylato ligands for the chemical vapor deposition of metal sulfides.

合成并表征了通式为Mo(SCR)₄（R = 甲基、乙基、丙基、苯基）的四（二硫代羧基）钼（IV）配合物，并将其作为用于气溶胶辅助化学气相沉积（AACVD）硫化钼薄膜的前驱体进行了预筛选。通过热重分析（TGA）和气相色谱 - 质谱联用（GC - MS）确定的配合物热行为适用于AACVD，尽管这些配合物对于传统的CVD鼓泡器系统挥发性不足。在500℃下，通过AACVD从Mo(SCMe)₄的甲苯溶液中生长出了硫化钼薄膜。通过掠入射X射线衍射（GIXRD）图谱对薄膜进行了表征，该图谱对应于沉积薄膜中的2H - MoS₂结构。X射线光电子能谱（XPS）和能谱分析（EDS）进一步证实了2H - MoS₂中的Mo - S键合。通过场发射扫描电子显微镜（FE - SEM）评估了薄膜的形态、垂直取向结构和厚度（2.54μm）。观察到了结晶态2H - MoS₂的拉曼E和A振动模式。这些结果证明了二硫代羧基配体在金属硫化物化学气相沉积中的应用。