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 ...
Over the past decade, carbon nanostructures (CNSs) have been widely used in a variety of biomedical applications. Examples are the use of CNSs for drug and protein delivery or in tools to locally dispense nucleic acids to fight tumor affections. CNSs were successfully utilized in diagnostics and in noninvasive and highly sensitive imaging devices thanks to their optical properties in the near infrared region. However, biomedical applications require a complete biocompatibility to avoid adverse reactions of the immune system and CNSs potentials for biodegradability. Water is one of the main constituents of the living matter. Unfortunately, one of the disadvantages of CNSs is their poor solubility. Surface functionalization of CNSs is commonly utilized as an efficient solution to both tune the surface wettability of CNSs and impart biocompatible properties. Grafting functional groups onto the CNSs surface consists in bonding the desired chemical species on the carbon nanoparticles via wet or dry processes leading to the formation of a stable interaction. This latter may be of different nature as the van Der Waals, the electrostatic or the covalent, the π-π interaction, the hydrogen bond etc. depending on the process and on the functional molecule at play. Grafting is utilized for multiple purposes including bonding mimetic agents such as polyethylene glycol, drug/protein adsorption, attaching nanostructures to increase the CNSs opacity to selected wavelengths or provide magnetic properties. This makes the CNSs a very versatile tool for a broad selection of applications as medicinal biochips, new high-performance platforms for magnetic resonance (MR), photothermal therapy, molecular imaging, tissue engineering, and neuroscience. The scope of this work is to highlight up-to-date using of the functionalized carbon materials such as graphene, carbon fibers, carbon nanotubes, fullerene and nanodiamonds in biomedical applications.
Effect of solution chemistry on the electropolymerization and the electrochemical properties of polypyrrole coatings on aluminum is studied by means of electrochemical techniques, scanning electron microscopy (SEM), and x-ray photoelectron spectroscopy. It is shown that the protection effect of the coating in long-term exposures and when exposed to more concentrated NaCl solutions depends on the chemistry of electropolymerization electrolyte. The results show that nitrate anions passivate the aluminum substrate during the electropolymerization process. The resulting coating is less prone to blistering in a NaCl solution and probably due to its higher electrochemical activity presents a higher anodic protection effect. The galvanic interaction of polypyrrole coating with aluminum in a NaCl solution is directly observed using focused ion beam-assisted SEM.
Cerium-based conversion coatings were deposited on high pressure die cast (HPDC) Al-Si alloys using an immersion method. Hydrogen peroxide and sodium chloride were added to the conversion solution to accelerate the coating formation and to understand its formation mechanism. These studies showed that the deposition of cerium hydroxide/oxide conversion layer starts from iron-rich intermetallic particles, which are located inside the eutectic region and then the coating growth continues to cover the entire alloy surface. This phenomenon passivates the active interfaces between iron-rich intermetallic particles and/or the eutectic silicon phase and the aluminum matrix, which are prone to localized corrosion in chloride ions containing environments. Accordingly, values of the total impedance in EIS measurements significantly increased for the treated substrates. Morphologies of the conversion coatings and the oxidation state of cerium compounds were found to be dependent on the composition of the solution and the presence of chloride ions and/or hydrogen peroxide. Aluminum alloy with higher silicon content showed a more active surface during immersion in the conversion solution. This makes it more difficult to be treated using aggressive conversion solutions.
Hybrid core–shell nanodiamond-gold nanoparticles were synthesized and characterized as a novel multifunctional material with tunable and tailored properties for multifunctional biomedical applications. The combination of nanostructured gold and nanodiamond properties afford new options for optical labeling, imaging, sensing, and drug delivery, as well as targeted treatment. ND@Au core–shell nanoparticles composed of nanodiamond (ND) core doped with Si vacancies (SiV) and Au shell were synthesized and characterized in terms of their biomedical applications. Several bioimaging modalities based on the combination of optical and spectroscopic properties of the hybrid nano-systems are demonstrated in cellular and developing zebrafish larvae models. The ND@Au nanoparticles exhibit isolated ND’s Raman signal of sp3 bonded carbon, one-photon fluorescence of SiV with strong zero-phonon line at 740 nm, two-photon excited fluorescence of nanogold with short fluorescence lifetime and strong absorption of X-ray irradiation render them possible imaging agent for Raman mapping, Fluorescence imaging, two-photon Fluorescence Lifetime Imaging (TP-FLIM) and high-resolution hard-X-ray microscopy in biosystems. Potential combination of the imaging facilities with other theranostic functionalities is discussed.
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