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 ...
In this paper, 6 different reduced graphene oxide (rGO) were prepared by a modified Hummers' method and reduced by thermochemical methods. rGO materials were intentionally prepared to obtain different BET and thickness and oxygen content maintaining constant the lateral size to compare its performance on thermoplastic polyurethane (TPU) matrix. Microstructure and the effect of the incorporation of rGO on the hardness and electrical properties of TPU were investigated. It has been studied the temperature and humidity dependence of the electrical conductivity and the sensitivity and the response time to humidity changes have been determined. Influence of the filler content, temperature and humidity on the Jonscher's universal power law (UPL) for ac conductivity vs frequency and its fitting parameters A and n were determined. It has been observed an anomalous behaviour (according to UPL) and a linear correlation between log A and n independently of the filler content, humidity and temperature, however there is an influence of the rGO used for the preparation of the composite. To study the transport mechanisms the experimental results were adjusted to the equation = 0 exp[-(TMott/T)] and the maximum adjustment for = 1/4 like other carbon nanocomposites however there is not an unequivocal behaviour.
Effects of chemical structure and morphology of graphene-related materials (GRMs) on melt processing and properties of GRM/polyamide-6 nanocomposites. Results in Materials, 7. p. 100105.
Two different types of graphene flakes were produced following solution processing methods and dispersed using shear mixing in a bifunctional (A) and a multifunctional (B) epoxy resin at a concentration of 0.8 and 0.6 wt% respectively. The graphene/epoxy resin mixtures were used to impregnate unidirectional carbon fibre tapes. These prepregs were stacked (seven plies) and cured to produce laminates. The interlaminar fracture toughness (mode-I) of the carbon fiber/graphene epoxy laminates with resin B showed over 56% improvement compared with the laminate without graphene. Single lap joints were prepared using the laminates as adherents and polyurethane adhesives (Sika 7666 and Sika 7888). The addition of graphene improved considerably the adhesion strength from 3.3 to 21 MPa (sample prepared with resin A and Sika 7888) highlighting the potential of graphene as a secondary filler in carbon fibre reinforced polymer composites.
Two different reduced graphene oxides (rGOs) with similar concentration of oxygen and defects and differences in exfoliation were prepared to produce the rGO/thermoplastic polyurethane nanocomposites by solution blending (SB) and melt compounding (MC). Morphology, electrical, and dielectric properties were studied. Large agglomerates have been observed for the composites produced by SB and discrete and low agglomerated rGO particles in the case on the composites produced by MC. These morphological differences justify the observations in hardness, electrical conductivity, and even in the dielectric properties. The composites do not follow Jonscher's universal power law (UPL) and a linear trend between UPL factors (Log A vs n) has been observed for composites produced by SB, however, no trend is observed in the composites produced by MC, being the first time observed. Differences in the tunneling effect and breakage of H-bonds within the polymer can be suggested from the dielectric relaxation characterization.
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