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

Jankowski, Maciej; Saedi, Mehdi; Porta, Francesco La; Manikas, Anastasios C.; Tsakonas, Christos; Cingolani, Juan Santiago; Andersen, Mie; Voogd, Marc de; Baarle, G. J. C. van; Reuter, Karsten; Galiotis, Costas; Renaud, Gilles; Konovalov, Oleg; Groot, Irene M. N.

doi:10.1021/acsnano.0c10377

Cited by 38 publications

(86 citation statements)

References 64 publications

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“…The XRR measurements were started when graphene covered the entire surface of the liquid copper. The growth coverage was monitored in real time with radiation-mode optical microscopy (Terasawa & Saiki, 2015;Jankowski et al, 2021).…”

Section: Xrr Measurements and Materialsmentioning

confidence: 99%

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X-ray reflectivity from curved surfaces as illustrated by a graphene layer on molten copper

Konovalov¹,

Belova²,

Porta³

et al. 2022

J Synchrotron Radiat

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The X-ray reflectivity technique can provide out-of-plane electron-density profiles of surfaces, interfaces, and thin films, with atomic resolution accuracy. While current methodologies require high surface flatness, this becomes challenging for naturally curved surfaces, particularly for liquid metals, due to the very high surface tension. Here, the development of X-ray reflectivity measurements with beam sizes of a few tens of micrometres on highly curved liquid surfaces using a synchrotron diffractometer equipped with a double crystal beam deflector is presented. The proposed and developed method, which uses a standard reflectivity θ–2θ scan, is successfully applied to study in situ the bare surface of molten copper and molten copper covered by a graphene layer grown in situ by chemical vapor deposition. It was found that the roughness of the bare liquid surface of copper at 1400 K is 1.25 ± 0.10 Å, while the graphene layer is separated from the liquid surface by a distance of 1.55 ± 0.08 Å and has a roughness of 1.26 ± 0.09 Å.

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Section: Xrr Measurements and Materialsmentioning

confidence: 99%

“…One of the examples of such measurement is our recent work on the growth of graphene on liquid metal catalysts (LMCats), i.e. molten copper, using chemical vapor deposition (CVD) (Jankowski et al, 2021). The graphene is grown on the molten copper surface using a dedicated reactor specially constructed for this purpose (Saedi et al, 2020).…”

Section: Introductionmentioning

confidence: 99%

X-ray reflectivity from curved surfaces as illustrated by a graphene layer on molten copper

Konovalov¹,

Belova²,

Porta³

et al. 2022

J Synchrotron Radiat

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“…Another technique based on instruments similar to conventional OM but focusing the thermal radiation has also been developed for visualizing 2D materials, which is called “radiation‐mode OM.“ [ 58 ] The radiation‐mode OM have been used to establish the in situ and real‐time observation on the growth of graphene on Cu during the CVD process. [ 58 , 59 ] At high temperature, both the thermal radiations from the graphene and the Cu substrate are strong so that sufficient contrast could be obtained depending on the difference in their emissivities. Using this technique, the growth mechanism of CVD graphene can be observed and the growing parameters can be optimized.…”

Section: Locating 2d Materialsmentioning

confidence: 99%

Optical Inspection of 2D Materials: From Mechanical Exfoliation to Wafer‐Scale Growth and Beyond

et al. 2021

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Optical inspection is a rapid and non-destructive method for characterizing the properties of two-dimensional (2D) materials. With the aid of optical inspection, in situ and scalable monitoring of the properties of 2D materials can be implemented industrially to advance the development and progress of 2D material-based devices toward mass production. This review discusses the optical inspection techniques that are available to characterize various 2D materials, including graphene, transition metal dichalcogenides (TMDCs), hexagonal boron nitride (h-BN), group-III monochalcogenides, black phosphorus (BP), and group-IV monochalcogenides. First, the authors provide an introduction to these 2D materials and the processes commonly used for their fabrication. Then they review several of the important structural properties of 2D materials, and discuss how to characterize them using appropriate optical inspection tools. The authors also describe the challenges and opportunities faced when applying optical inspection to recently developed 2D materials, from mechanically exfoliated to wafer-scale-grown 2D materials. Most importantly, the authors summarize the techniques available for largely and precisely enhancing the optical signals from 2D materials. This comprehensive review of the current status and perspective of future trends for optical inspection of the structural properties of 2D materials will facilitate the development of next-generation 2D material-based devices.

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“… Groot I. M. N. 34060320 ACS Nano 2021 15 9638 9648 . 4 Using real-time observations of growth of graphene on liquid copper, we are able to tailor the growth parameters such that very large single-crystalline graphene sheets can be produced. The growth is determined by an interplay of electrostatic interactions and capillary forces on liquid copper.…”

Section: Key Referencesmentioning

confidence: 99%

“…The Raman and X-ray reflectivity spectra of our graphene grown on liquid copper compare favorably to those of exfoliated graphene. 4 …”

Section: In Situ Reactor For Graphene Growth On Liquid Coppermentioning

confidence: 99%

Investigation of Active Catalysts at Work

Groot

2021

Acc. Chem. Res.

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Conspectus Even after being in business for at least the last 100 years, research into the field of (heterogeneous) catalysis is still vibrant, both in academia and in industry. One of the reasons for this is that around 90% of all chemicals and materials used in everyday life are produced employing catalysis. In 2020, the global catalyst market size reached $35 billion, and it is still steadily increasing every year. Additionally, catalysts will be the driving force behind the transition toward sustainable energy. However, even after having been investigated for 100 years, we still have not reached the holy grail of developing catalysts from rational design instead of from trial-and-error. There are two main reasons for this, indicated by the two so-called “gaps” between (academic) research and actual catalysis. The first one is the “pressure gap”, indicating the 13 orders of magnitude difference in pressure between the ultrahigh vacuum lab conditions and the atmospheric pressures (and higher) of industrial catalysis. The second one is the “materials gap”, indicating the difference in complexity between single-crystal model catalysts of academic research and the real catalysts, consisting of metallic nanoparticles on supports, promoters, fillers, and binders. Although over the past decades significant efforts have been made in closing these gaps, many steps still have to be taken. In this Account, I will discuss the steps we have taken at Leiden University to further our fundamental understanding of heterogeneous catalysis at the (near-)atomic scale. I will focus on bridging the pressure gap, though we are also working on closing the materials gap. Over the past years, we developed state-of-the-art equipment that is able to investigate the (near-)atomic-scale structure of the catalyst surface during the chemical reaction using several surface-science-based techniques such as scanning tunneling microscopy, atomic force microscopy, optical microscopy, and X-ray-based techniques (surface X-ray diffraction, grazing-incidence small-angle X-ray scattering, and X-ray reflectivity, in collaboration with ESRF). Simultaneously with imaging the surface, we can investigate the catalyst’s performance via mass spectrometry, enabling us to link changes in the catalyst structure to its activity, selectivity, or stability. Although we are currently investigating many industrially relevant catalytic systems, I will here focus the discussion on the oxidation of platinum during, for example, CO and NO oxidation, the NO reduction reaction on platinum, and the growth of graphene on liquid (molten) copper. I will show that to be able to obtain the full picture of heterogeneous catalysis, the ability to investigate the catalyst at the (near-)atomic scale during the chemical reaction is a must.

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

Cited by 38 publications

References 64 publications

X-ray reflectivity from curved surfaces as illustrated by a graphene layer on molten copper

X-ray reflectivity from curved surfaces as illustrated by a graphene layer on molten copper

Optical Inspection of 2D Materials: From Mechanical Exfoliation to Wafer‐Scale Growth and Beyond

Investigation of Active Catalysts at Work

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