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<p>Hybrid nanostructured materials have attracted significant attention due to their robust multifunctional properties. Among them, 2D@1D nanostructures are particularly promising. The rational design of such heterostructures requires synthesis routes that combine interfacial cleanliness, structural control, and real-time mechanistic insight. In this study, we report a solvent-free strategy for growing high-crystalline MoS<sub>2</sub> nanoflakes on single-walled carbon nanotubes (SWCNTs) using an integrated chemical vapor deposition/molecular beam epitaxy (CVD/MBE) platform coupled with operando X-ray photoelectron spectroscopy. This setup enables continuous monitoring of nucleation and growth under ultra-high vacuum, and allows atomically sharp interfaces. We achieved uniform coverage of SWCNT sidewalls with MoS<sub>2</sub> nanoflakes about 4-5 layers thick (~4 nm) and spanning areas exceeding 100 nm<sup>2</sup>. Operando XPS uncovers a stepwise growth pathway from sulfur adsorption on CNTs to Mo–S<sub>3</sub> cluster formation, and the subsequent transformation into crystalline 2H-MoS<sub>2</sub> domains. Complementary in-situ XPS validation confirms the high crystallinity, stoichiometry, and van der Waals interfacial coupling of the final heterostructure. The resulting heterostructures exhibit abundant exposed edge sites, strong interfacial coupling, and p-doping of SWCNTs without covalent disruption. This work establishes a versatile route for precision engineering of hybrid nanostructures while providing insights into their atomistic growth mechanisms.</p>

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Operando XPS monitoring of MoS2 nanoflake nucleation on carbon nanotubes via integrated CVD-MBE

  • 期刊论文

  • 出版模式：

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  • 发表日期：

    2026年4月28日

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  • Haifa Taoum,
  • Mariam Ezzedine,
  • Ileana Florea,
  • Costel-Sorin Cojocaru

摘要

Hybrid nanostructured materials have attracted significant attention due to their robust multifunctional properties. Among them, 2D@1D nanostructures are particularly promising. The rational design of such heterostructures requires synthesis routes that combine interfacial cleanliness, structural control, and real-time mechanistic insight. In this study, we report a solvent-free strategy for growing high-crystalline MoS2 nanoflakes on single-walled carbon nanotubes (SWCNTs) using an integrated chemical vapor deposition/molecular beam epitaxy (CVD/MBE) platform coupled with operando X-ray photoelectron spectroscopy. This setup enables continuous monitoring of nucleation and growth under ultra-high vacuum, and allows atomically sharp interfaces. We achieved uniform coverage of SWCNT sidewalls with MoS2 nanoflakes about 4-5 layers thick (~4 nm) and spanning areas exceeding 100 nm2. Operando XPS uncovers a stepwise growth pathway from sulfur adsorption on CNTs to Mo–S3 cluster formation, and the subsequent transformation into crystalline 2H-MoS2 domains. Complementary in-situ XPS validation confirms the high crystallinity, stoichiometry, and van der Waals interfacial coupling of the final heterostructure. The resulting heterostructures exhibit abundant exposed edge sites, strong interfacial coupling, and p-doping of SWCNTs without covalent disruption. This work establishes a versatile route for precision engineering of hybrid nanostructures while providing insights into their atomistic growth mechanisms.