Sonochemical preparation of carbon spheres

Spherical morphology of carbon with 150–400 nm size is produced by sonication (480 kHz, 2.5 W) of toluene with water under ambient conditions. Medium range of frequency and weak power of ultrasound is found to be the appropriate conditions for preparing the carbon spheres. Morphological and structural analysis of the product is carried out with TEM, SEM, elemental analysis, TGA, and FT-IR spectroscopy.     

Preparation and characterization of amphiphilic multi-walled carbon nanotubes

Multiwalled carbon nanotubes (MWCNTs, average diameter 8 nm) functionalized by N-vinyl pyrrolidone (NVP) were synthesized by radical polymerization and characterized by Fourier transform infrared and Raman spectroscopies, thermogravimetric analysis and transmission electron microscopy. These NVP–MWCNTs exhibit remarkable solubility in water, ethanol and dimethyl formamide. The polyvinyl pyrrolidone can be attached onto the surface of the MWCNTs and the degree of functionalization is affected by NVP content. The functionalization causes possible grafting reaction and solid physical coating between MWCNTs and PVP.     

Preparation and microwave characterization of submicrometer-sized hollow nickel spheres

The hollow structural submicrometer-sized nickel spheres were successfully fabricated by the autocatalytic reduction method. Because of the metallic and ferromagnetic behaviour of the nickel spheres, the low-density microspheres could obtain high dielectric constant and magnetic loss in microwave frequencies. The abrupt variation of the real part and the sharp peaks of the imaginary part of permittivity and permeability were observed for the micrometer-sized and nanometer-sized nickel hollow spheres. Reflection loss less than −25 dB were predicted over 11 GHz with a thickness of 1.5–2.0 mm.     

Realization, characterization and functionalization of lipidic wrapped carbon nanotubes

Mass-produced carbon nanotubes (CNTs) are strongly aggregated and highly hydrophobic, and processes to make them water soluble are required for biological applications. Both covalent and non-covalent strategies are pursued for obtaining stable, highly concentrated CNT aqueous dispersions. Covalent functionalization has the great disadvantage of producing an irreversible chemical modification of nanotubes, thus alterating their mechanical, chemical and electric properties. On the other hand, non-covalent functionalization is often obtained by employing surfactants that sensibly affect cell viability. Moreover, derivatization with biological moieties is often impossible through non-covalent CNT dispersion. This paper proposes a non-covalent dispersion of multi-wall CNT based on a lipidic mixture that can guarantee high concentration and high stability as well as high cytocompatibility. Moreover, CNTs wrapped with a lipid membrane are realized to demonstrate that the proposed CNTs can be functionalised with a dodecapeptide that specifically recognizes activated platelets without chemical modification of the nanotube itself.     

Purification of carbon nanotubes grown by thermal CVD

We show the results of a set of purifications on carbon nanotubes (CNT) by acid and basic treatments. CNTs were obtained by thermal decomposition of camphor at 850 °C in a CVD growth system, by means of a growth process catalyzed by iron clusters originating from the addition of ferrocene in the precursors mixture. The purification procedures involved HNO₃, H₂SO₄, HSO₃Cl and NaOH for different process temperatures.As-grown CNTs showed a consistent presence of metal catalyst (about 6 wt%), evidenced by TGA. The purification treatments led to a certain amount of opening of the CNT tips, with a consequent loss of metal catalyst encapsulated in tips. This is also confirmed by BET analysis, which showed an increase of the surface area density of CNT after the purification.FT-IR and XPS revealed the presence of carboxylic groups on the CNT surface chemically modified by the harsh environment of the purification process.Among the various treatments that have been tested, the 1:3 solution of nitric and sulphuric acid was the most effective in modifying the CNT surface and inducing the formation of functional groups.     

Biological functionalization and fluorescent imaging of carbon nanotubes

Biofunctionalization and manipulating of carbon nanotubes (CNTs) is important for biomedical research and application. Cy5 labeled goat anti-rabbit IgG (anti-IgG-Cy5) is chemically bonded to CNTs via a two-step process of diimide-activated amidation. This process can avoid the intermolecular connection of proteins. Fluorescent imaging of CNTs in aqueous solution has been demonstrated using anti-IgG-Cy5 immobilized CNTs (IgG-CNTs) as the model. The biologically functionalized carbon nanotubes (f-CNTs) in solution have been observed successfully using fluorescence microscopy. The fluorescent image of highly oriented f-CNTs is obtained at first time. The influencing factors on fluorescent imaging including oxidation duration, background noise and reactant concentration are discussed.     

非晶空心碳球的制备及生长机制

采用射频等离子体增强化学气相沉积技术,在CH4/H2的气氛中合成了非晶空心碳球.利用SEM,TEM,拉曼光谱对样品的形貌、成分和结构进行了表征.非晶空心碳球的直径在100～800nm之间,分布在弯曲的碳纳米管丛中.非晶空心碳球的生长机制可能为膨胀生长.     

Preparation and characterization of antibacterial Au/C core-shell composite

An environment-friendly oxidation-reduction method was used to prepare Au/C core-shell composite using carbon as core and gold as shell. The chemical structures and morphologies of Au/C core-shell composite and carbon sphere were characterized by X-ray diffraction, transmission electron microscope, energy dispersion X-ray spectrometry (EDS) and X-ray photoelectron spectroscopy (XPS). The antibacterial properties of the Au/C core-shell composite against Escherichia coli (E. coli), Staphylococcus aureus (S. aureus) and Candida albicans (C. albicans) were examined by the disk diffusion assay and minimal inhibition concentration (MIC) methods. In addition, antibacterial ability of Au/C core-shell composite was observed by atomic force microscope. Results demonstrated that gold homogeneously supported on the surface of carbon spheres without aggregation and showed efficient antibacterial abilities.     

One-pot, efficient functionalization of multi-walled carbon nanotubes with diamines by microwave method

Diamines are known to act as a medium to bind miscellaneous compounds to carbon nanotubes (CNT). However, they are commonly applied in a tedious manner. Here, multi-walled carbon nanotubes (MWCNTs) were functionalized by a series of diamine molecules (ethylenediamine, 1,6-hexamethylenediamine and 1,4-diaminobenzen) in a one-pot, rapid microwave-assisted method. Surface functionality groups and morphology of MWCNTs were analyzed by infrared spectroscopy, thermogravimetric analysis, Raman spectroscopy, scanning electron microscopy, and transmission electron microscopy. The results consistently confirmed the formation of diamines functionalities on MWCNTs, while the structure of MWCNT has remained relatively intact. This simple and efficient process may play an important role for realizing miscellaneous functionalization of CNTs.     

Preparation of anti-oxidative carbon fiber at high temperature

In this paper, carbon fibers with improved thermal stability and oxidation resistive properties were prepared and evaluated their physical performances under oxidation condition. Carbon fibers were coated with SiC particles dispersed in a polyacrylonitrile solution and then followed by pyrolyzed at 1400 °C to obtain the SiC nanoparticle deposition on the surface of the carbon fiber. The SiC coated carbon fiber showed extended oxidation resistive property as remaining 80-88% of the original weight even at high temperature 1000 °C under air, as compared with the control of zero weight at 600 °C. The effects of the coating conditions on the oxidation resistive properties of the coated fibers were studied in detail.     

Functionalization of carbon nanotubes with silver clusters

In this paper, an advanced method of one-step functionalization of single and multi walled carbon nanotubes (SWCNTs and MWCNTs) using γ-irradiation was described. Two synthesis procedures, related with different reduction species, were employed. For the first time, poly(vinyl alcohol) PVA is successfully utilized as a source to reduce silver (Ag) metal ions without having any additional reducing agents to obtain Ag nanoparticles on CNTs. The decoration of carbon nanotubes with Ag nanoparticles takes place through anchoring of (PVA) on nanotube's surface. Optical properties of as-prepared samples and mechanism responsible for the functionalization of carbon nanotubes were investigated using UV-vis and FTIR spectroscopy, respectively. Decorated carbon nanotubes were visualized using microscopic techniques: transmission electron microscopy and scanning tunneling microscopy. Also, the presence of Ag on the nanotubes was confirmed using energy dispersive X-ray spectroscopy. This simple and effective method of making a carbon nanotube type of composites is of interest not only for an application in various areas of technology and biology, but for investigation of the potential of radiation technology for nanoengineering of materials.     

Structural and surface features of multiwall carbon nanotube

We present the direct evidence of defective and disorder places on the surface of multiwall carbon nanotube (MWCNT), visualizing the presence of amorphous carbon at those sites. These defective surfaces being higher in energy are the key features of functionalization with different materials. The interaction of the π orbital electrons of different carbon atoms of adjacent layers is more at the bent portion, than that of regular portion of the CNT. Hence the tubular structure of the bent portion of nanotubes is spaced more than that of regular portion of the nanotubes, minimizing the stress.     

Preparation and characterization of biocompatible magnetic carbon nanotubes

Magnetic carbon nanotubes consisting of multi-wall carbon nanotubes (MWNTs) core and Fe₃O₄ shell were successfully prepared by in situ thermal decomposition of Fe(acac)₃ or FeCl₃ or Fe(CO)₅ in 2-pyrrolidone containing acid treated MWNTs at 240 °C with the protection of nitrogen gas. The samples were characterized by TEM, XRD, SEAD, XPS and superconducting quantum interference device. Also, their biocompatibility was compared with naked carbon nanotubes. The results showed that after coated with Fe₃O₄ nanoparticles, the obtained magnetic carbon nanotubes show superparamagnetic characteristic at room temperature, and their blocking temperature is about 80 K. The magnetic properties of the nanotubes are relevant to the content of magnetic particles, increasing content of magnetic nanoparticles leads to higher blocking temperature and saturation magnetization. The results of antimicrobial activities to bacterial cells (Escherichia coli) showed that the MWNTs have antimicrobial activity, while the magnetic nanotubes are biocompatible even with a higher concentration than that of MWNTs.     

Modification of polystyrene-based activated carbon spheres to improve adsorption of dibenzothiophene

Polystyrene-based activated carbon spheres (PACS) were modified with either air, HNO₃, (NH₄)₂S₂O₈, H₂O₂ or H₂ to improve their adsorption properties of dibenzothiophene (DBT). The texture and surface chemistry of PACS were characterized by N₂ adsorption, scanning electron microscopy (SEM), temperature-programmed desorption (TPD), X-ray photoelectron spectroscopy (XPS), acid-base titration and elemental analysis. The results showed that HNO₃ and (NH₄)₂S₂O₈ treatments introduced large amount of acidic groups such as carboxylic, lactones and anhydride groups, while air and H₂O₂ had relatively mild effects and introduced a small quantity of phenol, carbonyl and ether groups. In the HNO₃ treatment, the acidic groups might be fixed on the internal and external surface of PACS, which may act as active sites of adsorption, resulting in increase of the adsorption amount by 45%. Whereas H₂O₂ and (NH₄)₂S₂O₈ treatments might fix more oxygen-containing groups on the external surface, which may hinder DBT molecule enter into micropores, leading to rather lower adsorption capacity with the extent of oxidation. So, the concentration, distribution and types of the acidic functional groups are responsible for the removal of DBT.     

Synthesis and characterization of carbon nanotubes on carbon microfibers by floating catalyst method

In this paper, carbon nanotubes were synthesized on carbon microfibers by floating catalyst method with the pretreatment of carbon microfibers at the temperature of 1023 K, using C₂H₂ as carbon source and N₂ as carrier gas. The morphology and microstructure of carbon nanotubes were characterized by field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). The composition of carbon nanotubes was determined by energy dispersive X-ray spectroscopy (EDX). The results showed that the surface of treated carbon microfibers was thickly covered by carbon nanotubes with diameters of about 50 nm. EDX image indicated that the composition of carbon nanotubes was carbon. In comparison with the sample grown on untreated carbon microfibers surface, it was found that after carbon microfibers were boiled in the solution of sulfur acid and nitric acid (VH₂SO₄:VHNO₃ = 1:3) and immersed in the solution of iron nitrate and xylene, carbon nanotubes with uniform density can be grown on carbon microfibers surface. Based on the results, we concluded that the pretreatment of carbon microfibers had great effect on the growth of carbon nanotubes by floating catalyst method.     

Preparation and microwave absorption properties of electroless Co-P-coated nickel hollow spheres

Co-P-coated nickel hollow spheres (NHSs) were prepared by electroless plating technology. The morphology and component content of Co-P coating varies with the change of sodium citrate concentration in elctroless plating solution. And as phosphorus content increases in coatings, resulting in smaller grain, coercivity of microspheres decreases. The microwave absorption properties of spheres-wax composite were investigated in the range of 2-18 GHz. Both permittivity and permeability increase with an increase of cobalt content in coatings. For composite layer, a minimal reflection loss (RL, −36.9 dB) of was predicted at 8.1 GHz with a thickness of 3 mm.     

Ultrathin MnO2 nanosheets grown on hollow carbon spheres with enhanced capacitive performance

Ultrathin MnO₂ nanosheets grown on the surface of hollow carbon spheres (MnO₂/HCSs) were fabricated by the redox reaction between carbon spheres with KMnO₄ in aqueous solution. Due to the porous structure and large amounts of active sites, MnO₂/HCSs exhibit excellent capacitive performance with 227.5 F g⁻¹ at 1 A g⁻¹. After 5000 cycles, the capacity retention of MnO₂/HCSs remains 96%, indicating its good cycling stability. These results demonstrate that MnO₂/HCSs are promising supercapacitor electrode material and this work provide a facile method for growth of ultrathin MnO₂ nanosheets on carbon substrate.     

Fabrication and characterization of Pd/Ag alloy hollow spheres by the solvothermal method

Pd/Ag alloy hollow spheres have been synthesized in ethylene glycol solution by the solvothermal method and have been characterized extensively. TEM results have revealed the formation of Pd/Ag hollow spheres. Moreover, HRTEM results confirmed the formation of Pd/Ag alloy spheres, where the lattice fringe spacing is 0.229 nm corresponding to the (111) plane of Pd/Ag alloy. SEM, XRD and UV–vis results have further suggested the formation of alloy hollow spheres. The preliminary results showed the reaction time may be an importance factor influencing the formation of Pd/Ag alloy hollow spheres.     

An efficient route towards the covalent functionalization of single walled carbon nanotubes

A simple and efficient method of chemical functionalization of both single and multiwalled carbon nanotubes has been discussed to give enhanced water solubility by rapidly and efficiently generating an appreciable amount of hydrophilic functional groups using microwave radiation. Surface functionalization containing more than 30 wt% of oxygen has been achieved, resulting into solubility of 2–5 mg/mL. Further covalent functionalization of such soluble SWNTs provides a remarkable degree of aniline functionalization through amidation, where the formation of polyaniline has been avoided. Functionalization of SWNTs is confirmed by techniques like electron microscopy, Fourier transform infrared spectroscopy, thermogravimetry, Raman spectroscopy, cyclic voltammetry and impedance spectroscopy. Electrochemical analysis suggests an enhanced double layer capacitance (110 F/g) of nanotubes after microwave treatment. Aniline functionalization of SWNTs shows possible variations on the nanotube topography with concomitant formation of a dynamic polymer layer on the nanotube surface.     

Effects of different carbon precursors on synthesis of multiwall carbon nanotubes: Purification and Functionalization

Cyclohexanol and xylene were used as carbon precursors, for synthesis of multiwall carbon nanotubes (MWCNTs) arrays in a CVD system at temperature of 750 °C, using nitrogen as carrier gas and ferrocene as catalyst. Different characterization methods were employed to compare the MWCNTs structure synthesized by these two precursors. All scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermal gravimetric analysis (TGA) and Raman spectroscopy results illustrated that using cyclohexanol could significantly reduce formation of amorphous carbon and catalyst particles in the as-grown CNTs. The less amorphous carbon can be attributed to in situ oxidation in presence of oxygen atom of cyclohexanol. Characterizations showed that MWCNTs with high purity could be obtained using cyclohexanol as carbon precursor. The as-grown MWCNTs were purified by oxidation and acid treatment. Characterization of the purified MWCNTs using HNO₃/H₂SO₄ (1/3 or 1/1), 8 M HCl or 8 M HNO₃ was carried out. The results showed that 8 M HNO₃ could be considered as the best chemical to obtain more pure MWCNTs, less amorphous and metal particles and less damaged MWCNTs. The Raman spectroscopy results demonstrated that HNO₃/H₂SO₄ (1/3) treatment could more disorder the MWCNTs structure and this was attributed to the bigger destroying effect of this acid treatment. Furthermore, the TEM analysis of MWCNTs before and after acid treatment revealed that acid treatment could remove encapsulated catalyst particles. The FTIR analysis illustrated that purification of the MWCNTs with nitric acid could connect the functional groups onto the outer surface of MWCNTs and this resulted in more dispersion of the MWCNTs in water.