Development of a reactor for the in situ monitoring of 2D materials growth on liquid metal catalysts, using synchrotron X-ray scattering, Raman spectroscopy, and optical microscopy

Mehdi Saedi , J M de Voogd , A Sjardin , A Manikas , C Galiotis , M Jankowski , Gilles Renaud (1, 2) , F La Porta , O Konovalov , G J C van Baarle , I M N Groot

1 NRS - Nanostructures et Rayonnement Synchrotron
2 MEM - Modélisation et Exploration des Matériaux

Liquid metal catalysts (LMCats) (e.g. molten copper) can provide a new mass-production method for two-dimensional materials (2DMs) (e.g. graphene) with significantly higher quality and speed, and lower energy and material consumption. To reach such technological excellence, the physicochemical properties of LMCats, and the growth mechanisms of 2DMs on LMCats should be investigated. Here we report the development of a CVD reactor which allows the investigation of ongoing chemical reactions on the surface of a molten metal at elevated temperatures and under reactive conditions. The surface of the molten metal is monitored simultaneously using synchrotron X-ray scattering, Raman spectroscopy, and optical microscopy, thereby providing complementary information about the atomic structure and chemical state of the surface. To enable in situ characterization on a molten substrate at high temperatures (e.g. ~1370 K for copper), the optical and X-rays windows need to be protected from the evaporating LMCat, reaction products, and intense heat. This has been achieved by creating specific gas-flow patterns inside the reactor. The optimized design of the reactor has been achieved using multi-physics COMSOL simulations, which take into account the heat transfer, fluid dynamics, and transport of LMCat vapor inside the reactor. The setup has been successfully tested and is currently used to investigate the chemical vapor deposition (CVD) growth of graphene on the surface of molten copper under pressures ranging from medium vacuum up to atmospheric pressure.

Domaines: Chimie-Physique [physics.chem-ph]

Mehdi Saedi, J M de Voogd, A Sjardin, A Manikas, C Galiotis, et al.. Development of a reactor for the in situ monitoring of 2D materials growth on liquid metal catalysts, using synchrotron X-ray scattering, Raman spectroscopy, and optical microscopy. Review of Scientific Instruments, 2020, 91 (1), ⟨10.1063/1.5110656⟩. ⟨hal-02491504⟩