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Register a new userRapid CVD growth of millimetre-sized single crystal graphene using a cold-wall reactor
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In this work we present a simple pathway to obtain large single-crystal graphene on copper (Cu) foils with high growth rates using a commercially available cold-wall chemical vapour deposition (CVD) reactor. We show that graphene nucleation density is drastically reduced and crystal growth is accelerated when: i) using ex-situ oxidised foils; ii) performing annealing in an inert atmosphere prior to growth; iii) enclosing the foils to lower the precursor impingement flux during growth. Growth rates as high as 14.7 and 17.5 micrometers per minute are obtained on flat and folded foils, respectively. Thus, single-crystal grains with lateral size of about one millimetre can be obtained in just one hour. The samples are characterised by optical microscopy, scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy as well as selected area electron diffraction (SAED) and low-energy electron diffraction (LEED), which confirm the high quality and homogeneity of the films. The development of a process for the quick production of large grain graphene in a commonly used commercial CVD reactor is a significant step towards an increased accessibility to millimetre-sized graphene crystals.
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Recently, hexagonal boron nitride (h-BN) has been shown to act as an ideal substrate to graphene by greatly improving the material transport properties thanks to its atomically flat surface, low interlayer electronic coupling and almost perfect reticular matching. Chemical vapour deposition (CVD) is presently considered the most scalable approach to grow graphene directly on h-BN. However, for the catalyst-free approach, poor control over the shape and crystallinity of the graphene grains and low growth rates are typically reported. In this work we investigate the crystallinity of differently shaped grains and identify a path towards a real van der Waals epitaxy of graphene on h-BN by adopting a catalyst-free CVD process. We demonstrate the polycrystalline nature of circular-shaped pads and attribute the stemming of different oriented grains to airborne contamination of the h-BN flakes. We show that single-crystal grains with six-fold symmetry can be obtained by adopting high hydrogen partial pressures during growth. Notably, growth rates as high as 100 nm/min are obtained by optimizing growth temperature and pressure. The possibility of synthesizing single-crystal graphene on h-BN with appreciable growth rates by adopting a simple CVD approach is a step towards an increased accessibility of this promising van der Waals heterostructure.
A foundation of the modern technology that uses single-crystal silicon has been the growth of high-quality single-crystal Si ingots with diameters up to 12 inches or larger. For many applications of graphene, large-area high-quality (ideally of single-crystal) material will be enabling. Since the first growth on copper foil a decade ago, inch-sized single-crystal graphene has been achieved. We present here the growth, in 20 minutes, of a graphene film of 5 x 50 cm2 dimension with > 99% ultra-highly oriented grains. This growth was achieved by: (i) synthesis of sub-metre-sized single-crystal Cu(111) foil as substrate; (ii) epitaxial growth of graphene islands on the Cu(111) surface; (iii) seamless merging of such graphene islands into a graphene film with high single crystallinity and (iv) the ultrafast growth of graphene film. These achievements were realized by a temperature-driven annealing technique to produce single-crystal Cu(111) from industrial polycrystalline Cu foil and the marvellous effects of a continuous oxygen supply from an adjacent oxide. The as-synthesized graphene film, with very few misoriented grains (if any), has a mobility up to ~ 23,000 cm2V-1s-1 at 4 K and room temperature sheet resistance of ~ 230 ohm/square. It is very likely that this approach can be scaled up to achieve exceptionally large and high-quality graphene films with single crystallinity, and thus realize various industrial-level applications at a low cost.
Diamond displays a large variety of luminescence centers which define its optical properties and can be either created or modified by irradiation. The main purpose of the present work is to study the radiation hardness of several of such centers in homoepitaxial single crystal CVD diamond by following the evolution of photoluminescence and ionoluminescence upon 2 MeV proton irradiation. Luminescence decays were observed with values of the fluence at half of the starting luminescence (F1/2) of the order of 1014 cm-2. The 3H center displayed a non monotonic behavior, with a growing behavior and a subsequent decay with a rather high F1/2 value (in the order of few 1016 cm-2), maintaining at the highest fluences an intensity significantly higher than the blue A-band. A simple model based on a double-exponential trend was defined to fit with satisfactory accuracy the evolution of the 3H center. Several PL centers (namely: 3H, TR12, 491 nm, 494 nm) exhibited clear correlations and anti-correlations in their fluence dependences, which were considered in the attempt to acquire some insight into their possible alternative attributions.
Growing large-area single-crystal monolayers is the holy grail of graphene synthesis. In this work, the efficiency of graphene growth and the quality of their continuous films are explored through the time evolution of individual domains and their surface coverage on the substrate. Our phase-field modeling results and experimental characterization clearly demonstrate the critical roles of the deposition flux, edge-reaction kinetics and the surface diffusion of active carbon sources in modulating the pattern evolution and rate of growth. The contrast in edge-kinetics-limited and surface-diffusion-limited regimes is remarkable, which can be characterized by the evolution of domain patterns and considered as an indicator of the growth regime. Common features exist in these two regimes, showing that the growth rate scales with time as t2 in the early stage of growth and is regime-independent, which is explained by the coarsen profiles of carbon concentration for both the compact and dendritic domains. The rate decays rapidly in the final stage of growth due to the competition between neighboring domains on the limited carbon sources diffusing on the substrate, which is highly regime-sensitive and extremely low in the surface-diffusion-limited regime with narrow gaps between the domains to be filled. Based on these findings, synthesis strategies to improve the growth efficiency and film quality are discussed.
We have used Low Energy Electron Microscopy (LEEM) and Photo Emission Electron Microscopy (PEEM) to study and improve the quality of graphene films grown on Ir(111) using chemical vapor deposition (CVD). CVD at elevated temperature already yields graphene sheets that are uniform and of monatomic thickness. Besides domains that are aligned with respect to the substrate, other rotational variants grow. Cyclic growth exploiting the faster growth and etch rates of the rotational variants, yields films that are 99 % composed of aligned domains. Precovering the substrate with a high density of graphene nuclei prior to CVD yields pure films of aligned domains extending over millimeters. Such films can be used to prepare cluster-graphene hybrid materials for catalysis or nanomagnetism and can potentially be combined with lift-off techniques to yield high-quality, graphene based electronic devices.
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