Fullerene/carbon nanotube preparation

The most widely used method of fullerene and carbon nanotube preparation is an arc discharge in a buffer gas. Helium is usually applied as the gas. Argon is more widespread and cheap gas than helium. However the fullerene yield is less than 2 % with that gas whereas in a helium arc discharge it is about ten times greater. We have worked out an effective method of small quantity fullerene preparation by means of an argon arc discharge [1-3]. This report informs about the further investigation in this direction. 

Carbon nanotubes prepared by several methods are mixed with nanoparticles, amorphous carbon, fullerenes, and other contaminants [1576]. Nanotubes isolated from the mixture contain single-walled (SWNT) as well as multiwalled (MWNT) nanotubes. In general, the diameter of a SWNT is on the order of several nanometers, but the length can be several microns. Thus far, spectroscopic (mainly Raman) studies have been focused on SWNTs of small diameters (<2nm) that become metallic or semiconducting depending on their diameter and chirality. Chemical and physical... 

PREPARATION AND CHARACTERIZATION OF FULLERENES, CARBON NANOTUBES, AND CARBON ONIONS... 

Regarding a historical perspective on carbon nanotubes, very small diameter (less than 10 nm) carbon filaments were observed in the 1970 s through synthesis of vapor grown carbon fibers prepared by the decomposition of benzene at 1100°C in the presence of Fe catalyst particles of 10 nm diameter [11, 12]. However, no detailed systematic studies of such very thin filaments were reported in these early years, and it was not until lijima s observation of carbon nanotubes by high resolution transmission electron microscopy (HRTEM) that the carbon nanotube field was seriously launched. A direct stimulus to the systematic study of carbon filaments of very small diameters came from the discovery of fullerenes by Kroto, Smalley, and coworkers [1], The realization that the terminations of the carbon nanotubes were fullerene-like caps or hemispheres explained why the smallest diameter carbon nanotube observed would be the same as the diameter of the Ceo molecule, though theoretical predictions suggest that nanotubes arc more stable than fullerenes of the same radius [13]. The lijima observation heralded the entry of many scientists into the field of carbon nanotubes, stimulated especially by the un-... 

In the theoretical carbon nanotube literature, the focus is on single-wall tubules, cylindrical in shape with caps at each end, such that the two caps can be joined together to form a fullerene. The cylindrical portions of the tubules consist of a single graphene sheet that is shaped to form the cylinder. With the recent discovery of methods to prepare single-w alled nanotubes[4,5), it is now possible to test the predictions of the theoretical calculations. 

Carbon nanotubes have the same range of diameters as fullerenes, and are expeeted to show various kinds of size effeets in their struetures and properties. Carbon nanotubes are one-dimensional materials and fullerenes are zero-dimensional, whieh brings different effects to bear on their structures as well as on their properties. A whole range of issues from the preparation, structure, properties and observation of quantum effeets in carbon nanotubes in eomparison with 0-D fullerenes are diseussed in this book. 

Another important group of fullerene-related compounds are the carbon nanotubes, the reference compounds of the carbon nano-science. They may be obtained by convenient variations of the preparation procedure mentioned. These are long tubular fullerenes with a concentric shell structure a few nanometres wide and often capped with C60-like hemisphere or faceted tips. They are mechanically very strong and either metallic conducting or semiconducting types have been obtained. 

The number of studies on the health effects of fullerenes and carbon nanotubes is rapidly increasing. However, the data on their toxicity are often mutually contradictory. For example, the researchers from universities of Rice and Georgia (USA) found that in aqueous fullerene solutions colloidal nano-C particles were formed, which even at low concentration (approximately 2 molecules of fullerene per 108 molecules of water) negatively influence the liver and skin cells [17-19]. The toxicity of this nano-C aqueous dispersion was comparable to that of dioxins. In another smdy, however, it was shown that fullerene had no adverse effects and, on the contrary, had anti-oxidant activity [20]. Solutions of prepared by a variety of methods up to 200 mg/mL were not cytotoxic to a number of cell types [21]. The contradiction between the data of different authors could be explained by different nano-C particles composition and dispersion used in research. 

The physical-chemical properties of a synthetic gallophosphate molecular sieve, the 30-A supercage cloverite , have been assessed [18]. Instead of attempting to list the burgeoning number of fullerene publications, attention is drawn to the formation and characterization of fullerene-like nanocrystals of tungsten disulfide [19,20]. Preparation, characterization and utilization of carbon nanotubes have been the subject of a number of reports from several laboratories [21-27]. 

The discovery of fullerenes in 1985 led to the era of nanomaterials.1 The three-dimensional geometry of these molecules as well as their unique properties distinguishes them from conventional molecules encountered in organic chemistry. Due to recent discoveries in this field, the horizons of this area have broadened to encompass various new molecules such as endohedral fullerenes, nanotubes, carbon nanohorns, and carbon nano-onions. This chapter discusses the electrochemical behavior of some of these carbon nanoparticles with special emphasis on endohedral fullerenes. Since a large number of fullerene derivatives have been prepared and their various electrochemical studies in different solvents and electrolytes have been reported, the electrochemistry of these derivatives is beyond the scope of this text.2 3 Among the other carbon nanoparticles, the electrochemistry of derivatives of carbon nanotubes has been reported. These studies have been highlighted in the final part of the chapter. 

This review describes the preparation, characterization, and properties of all nonpolymeric complexes that contain a metal removed from the fullerene also are included. The article does not cover the essentially ionic fullerides MmC (4) or the endohedral metallofullerenes MmC (8), which have been reviewed previously. The extended fullerenes, or so-called carbon nanotubes, which have hollow centers and can be filled with metal salts, also are not discussed. The majority of complexes involve 7r-bonds and, apart from alkyl lithium fullerides, the potentially useful synthetic area of o- complexes has not been explored. Table I shows the occurrence of metal-bound adducts across the periodic table. 

Research in graphite intercalates has paved the way for significant current interest in intercalation compounds of the fullerenes (Box 7.1) and carbon nanotubes, which represent wrapped up versions of graphite sheets. Graphite intercalation compounds have been prepared with intercalated fullerenes and nanotubes. We will return to carbon nanotube chemistry in Chapter 15. 

Five years after the discovery of fullerenes, Iijima reported in 19911 a novel form of organized carbon which consists of hollow cylindrical structures, a few nanometers in diameter and some micrometers long. Although hollow carbon nanofibers had been prepared for several decades, their walls had never been resolved by High-Resolution Transmission Electron Microscopy (HRTEM). These HRTEM images allowed Iijima to conclude that the walls of the so-called multi-walled carbon nanotubes (MWCNTs) are made up of several concentric cylinders, each being formed by a graphene sheet rolled... 

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