We present an overview of the main techniques for production and processing of graphene and related materials (GRMs), as well as the key characterization procedures. We adopt a ‘hands-on’ approach, providing practical details and procedures as derived from literature as well as from the authors’ experience, in order to enable the reader to reproduce the results. Section is devoted to ‘bottom up’ approaches, whereby individual constituents are pieced together into more complex structures. We consider graphene nanoribbons (GNRs) produced either by solution processing or by on-surface synthesis in ultra high vacuum (UHV), as well carbon nanomembranes (CNM). Production of a variety of GNRs with tailored band gaps and edge shapes is now possible. CNMs can be tuned in terms of porosity, crystallinity and electronic behaviour. Section covers ‘top down’ techniques. These rely on breaking down of a layered precursor, in the graphene case usually natural crystals like graphite or artificially synthesized materials, such as highly oriented pyrolythic graphite, monolayers or few layers (FL) flakes. The main focus of this section is on various exfoliation techniques in a liquid media, either intercalation or liquid phase exfoliation (LPE). The choice of precursor, exfoliation method, medium as well as the control of parameters such as time or temperature are crucial. A definite choice of parameters and conditions yields a particular material with specific properties that makes it more suitable for a targeted application. We cover protocols for the graphitic precursors to graphene oxide (GO). This is an important material for a range of applications in biomedicine, energy storage, nanocomposites, etc. Hummers’ and modified Hummers’ methods are used to make GO that subsequently can be reduced to obtain reduced graphene oxide (RGO) with a variety of strategies. GO flakes are also employed to prepare three-dimensional (3d) low density structures, such as sponges, foams, hydro- or aerogels. The assembly of flakes into 3d structures can provide improved mechanical properties. Aerogels with a highly open structure, with interconnected hierarchical pores, can enhance the accessibility to the whole surface area, as relevant for a number of applications, such as energy storage. The main recipes to yield graphite intercalation compounds (GICs) are also discussed. GICs are suitable precursors for covalent functionalization of graphene, but can also be used for the synthesis of uncharged graphene in solution. Degradation of the molecules intercalated in GICs can be triggered by high temperature treatment or microwave irradiation, creating a gas pressure surge in graphite and exfoliation. Electrochemical exfoliation by applying a voltage in an electrolyte to a graphite electrode can be tuned by varying precursors, electrolytes and potential. Graphite electrodes can be either negatively or positively intercalated to obtain GICs that are subsequently exfoliated. We also discuss the materials that can be amenable to exfoliation, by ...
An environmentally benign and scalable route for the production of gram scale quantities of nitrogen-doped graphene using a downstream microwave plasma source is reported. Simultaneous reduction and doping of graphene oxide is achieved and the process negates the need for high temperatures and toxic solvents associated with existing methods. This gas-phase low temperature process is completely dry and, thus, minimises re-aggregation of graphene flakes which is typically associated with liquid phase reduction methods. The resulting material has many potential uses, particularly in electrochemical energy.
Mixed Mn/Ru oxide thermally prepared electrodes using different compositions of Mn and Ru precursor salts have been fabricated on Ti supports via thermal decomposition at two annealing temperatures. Subsequently, the oxygen evolution reaction (OER) activities of these electrodes were determined. A majority of the mixed Mn/Ru catalysts are highly active for the OER, exhibiting lower overpotential values compared to those of the state-of-the-art RuO 2 and IrO 2 type materials, when measured at a current density of 10 mA cm −2 . These Mn/Ru oxide materials are also cheaper to produce than the aforementioned platinum group materials, therefore rendering the Mn/Ru materials more practical and economical. The Mn/Ru catalysts are also evaluated with respect to their Tafel slopes and turnover frequency numbers. Interestingly, scanning electron microscopy reveals that the morphologies of the electrodes change to a mud-cracked morphology, similar to that of the RuO 2 , with minimal amounts of the Ru precursor salt added to the Mn salt. Fourier transform infrared spectroscopy and X-ray diffraction show that the Mn material fabricated in this study at the two annealing temperatures is largely Mn 3 O 4 , while the Ru material is predominately RuO 2 . X-ray photoelectron spectroscopy was also used to investigate the Mn and Ru composition ratios in each of the films.
We report on an adjustable process for chemical vapour deposition of thin films of pyrolytic carbon on inert substrates using an acetylene feedstock. Through modification of the reaction parameters control over film thickness and roughness is attained. These conducting films can be deposited in a conformal fashion, with thicknesses as low as 5 nm and a surface roughness of less than 1 nm. The highly reliable, cost effective and scalable synthesis may have a range of applications in information and communications technology and other areas. Raman and X-ray photoelectron spectroscopies, as well as high resolution transmission electron microscopy are used to investigate the composition and crystallinity of these films. The suitability of these films as electrodes in transparent conductors is assessed through a combination of absorbance and sheet resistance measurements. The films have a resistivity of ~ 2 × 10-5 m but absorb strongly in the visible range. The electrochemical properties of the films are investigated and are seen to undergo a marked improvement following exposure to O 2 or N 2 plasmas, making them of interest as electrochemical electrodes.
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