In situ kinetic studies of CVD graphene growth by reflection spectroscopy

Tsakonas, Christos; Manikas, Anastasios C.; Andersen, Mie; Dimitropoulos, Marinos; Galiotis, Costas

doi:10.1016/j.cej.2021.129434

Cited by 13 publications

(14 citation statements)

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“…In general, even in the case of solid catalysts, there are limited reports on real-time observation of graphene growth, with notable examples of those employing radiation-mode optical microscopy, 31 environmental scanning electron microscopy, 32 or in situ reflectance spectroscopy. 33 However, on liquid catalysts, and contrary to the ultrahigh vacuum 34 and low-pressure 32 CVD on solid substrates, the lack of precise, multiscale in situ techniques enabling direct feedback on the growth parameters of atmospheric pressure CVD (including temperature, gas composition, and pressures), has led primarily to empirical recipes. Such recipes intrinsically suffer from a limited understanding of the graphene formation process and low reproducibility of the product due to the complex and stochastic nature of the growth phenomena.…”

Section: Introductionmentioning

confidence: 99%

“…Several examples of graphene growth on LMCats with different morphologies have been reported, and intense efforts have been made to optimize the CVD process. In general, even in the case of solid catalysts, there are limited reports on real-time observation of graphene growth, with notable examples of those employing radiation-mode optical microscopy, environmental scanning electron microscopy, or in situ reflectance spectroscopy . However, on liquid catalysts, and contrary to the ultrahigh vacuum and low-pressure CVD on solid substrates, the lack of precise, multiscale in situ techniques enabling direct feedback on the growth parameters of atmospheric pressure CVD (including temperature, gas composition, and pressures), has led primarily to empirical recipes.…”

Section: Introductionmentioning

confidence: 99%

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Real-Time Multiscale Monitoring and Tailoring of Graphene Growth on Liquid Copper

et al. 2021

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The synthesis of large, defect-free two-dimensional materials (2DMs) such as graphene is a major challenge toward industrial applications. Chemical vapor deposition (CVD) on liquid metal catalysts (LMCats) is a recently developed process for the fast synthesis of high-quality single crystals of 2DMs. However, up to now, the lack of in situ techniques enabling direct feedback on the growth has limited our understanding of the process dynamics and primarily led to empirical growth recipes. Thus, an in situ multiscale monitoring of the 2DMs structure, coupled with a real-time control of the growth parameters, is necessary for efficient synthesis. Here we report real-time monitoring of graphene growth on liquid copper (at 1370 K under atmospheric pressure CVD conditions) via four complementary in situ methods: synchrotron X-ray diffraction and reflectivity, Raman spectroscopy, and radiation-mode optical microscopy. This has allowed us to control graphene growth parameters such as shape, dispersion, and the hexagonal supra-organization with very high accuracy. Furthermore, the switch from continuous polycrystalline film to the growth of millimeter-sized defect-free single crystals could also be accomplished. The presented results have far-reaching consequences for studying and tailoring 2D material formation processes on LMCats under CVD growth conditions. Finally, the experimental observations are supported by multiscale modeling that has thrown light into the underlying mechanisms of graphene growth.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Real-Time Multiscale Monitoring and Tailoring of Graphene Growth on Liquid Copper

et al. 2021

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“…The most straightforward information obtained via in situ techniques is the growth rate and its dependence on the temperature, gas flow rate, precursor, substrate, and so on. 47,[59][60][61][71][72][73][74][75][76][77][78] In 2015, the growth and etching of graphene on Cu substrate were observed by the radiation-mode optical microscopy (Rad-OM). Bright patches of graphene grains were clearly recognized (Fig.…”

Section: Imaging Of the Growth Ratementioning

confidence: 99%

Progress on the in situ imaging of growth dynamics of two-dimensional materials

Zhu

Wang

et al. 2023

Nanoscale

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“…Broadband reflectometry has been demonstrated effective for in situ measurement of film thickness and monitoring growth of many types of semitransparent films from ALD oxides ( Figure ) [ 58 ] to CVD graphene. [ 59 ] Most studies demonstrate spectroscopic broadband reflectometry of stationary targets at different intervals of the growth/deposition process. But the method is effective for moving targets if the distance from the sensor optics to the target is held constant.…”

Section: Inline Roll‐to‐roll Metrology Techniquesmentioning

confidence: 99%

“…(Figure 7) [58] to CVD graphene. [59] Most studies demonstrate spectroscopic broadband reflectometry of stationary targets at different intervals of the growth/deposition process. But the method is effective for moving targets if the distance from the sensor optics to the target is held constant.…”

Section: Broadband Reflectometrymentioning

confidence: 99%

Real‐Time Metrology for Roll‐To‐Roll and Advanced Inline Manufacturing: A Review

Maize

Cakmak

et al. 2022

Adv Materials Technologies

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Roll‐to‐Roll (R2R) manufacturing is changing how state‐of‐the‐art technology is made. Roll‐to‐Roll is part of a family of advanced scalable inline manufacturing techniques that make traditional and state‐of‐the‐art products at high yield and reduced cost. R2R manufacturing has grown rapidly and is fundamental to several advanced technologies such as functional materials and films, sensors for medicine, biology, and environment monitoring, energy harvesting devices, and flexible electronics. Advantages of R2R manufacturing include ease of machine design, adaptability to a wide range of additive processing methods, and very high throughput. To keep up with advances in R2R manufacturing, novel methods have emerged to measure important product metrics (thickness, roughness, conductivity) and monitor quality (uniformity, defects) inline and in real‐time. This review provides an overview of the state‐of‐the‐art for real‐time inline metrology and quality control in modern R2R manufacturing. The survey considers both established inline metrology techniques such as line‐scan imaging and reflectometry, and techniques recently adapted or that show promise for real‐time inline R2R metrology such as ellipsometry, hyper‐spectral imaging, and Raman spectroscopy.

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In situ kinetic studies of CVD graphene growth by reflection spectroscopy

Cited by 13 publications

References 54 publications

Real-Time Multiscale Monitoring and Tailoring of Graphene Growth on Liquid Copper

Real-Time Multiscale Monitoring and Tailoring of Graphene Growth on Liquid Copper

Progress on the in situ imaging of growth dynamics of two-dimensional materials

Real‐Time Metrology for Roll‐To‐Roll and Advanced Inline Manufacturing: A Review

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