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 ...
Complex core@shell and core@shell@shell nanoparticles are systems that combine the functionalities of the inner core and outer shell materials together with new physico-chemical properties originated by their low (nano) dimensionality. Such nanoparticles are of prime importance in the fast growing field of nanotechnology as building blocks for more sophisticated systems and a plethora of applications. Here, it is shown that although conceptually simple a modified gas aggregation approach allows the one-step generation of well-controlled complex nanoparticles. In particular, it is demonstrated that the atoms of the core and the shell of the nanoparticles can be easily inverted, avoiding intrinsic constraints of chemical methods.
We present a bottom-up fabrication route based on the sputtering gas aggregation source that allows the generation of nanoparticles with controllable and tunable chemical composition while keeping the control of the cluster size. We demonstrate that the chemical composition of the particles can be monitored by the individual adjustment of the working parameters of the magnetrons inserted in a gas aggregation zone. Such control of the parameters leads to a fine control of the ion density of each target material and hence to the control of the chemical composition of the nanoparticles. In particular, we show through X-ray photoemission, atomic force microscopy, and high-resolution transmission electron microscopy that it is possible to generate bimetallic (AgAu) and trimetallic (AgAuPd) alloy nanoparticles with well-defined and tunable stoichiometries from three targets of pure Ag, Au, and Pd. The proposed route for the generation of nanoparticles opens new possibilities for the fabrication of nanoparticles using a physical method that, for some applications, could be complementary to the chemical methods.
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