A new method of preparing single-walled carbon nanotubes

A novel method of purification for single-walled carbon nanotubes, prepared by an arc-discharge method, is described. The method involves a combination of acid washing followed by high temperature hydrogen treatment to remove the metal nanoparticles and amorphous carbon present in the as-synthesized singlewalled carbon nanotubes. The purified single-walled carbon nanotubes have been characterised by low-angle X-ray diffraction, electron microscopy, thermo-gravi-metric analysis and Raman spectroscopy. Dedicated to Professor C N R Rao on his 70th birthday     

Low-temperature growth of single-walled carbon nanotubes by water plasma chemical vapor deposition

Preferential growth of pure single-walled carbon nanotubes (SWNTs) over multi-walled carbon nanotubes (MWNTs) was demonstrated at low temperature by water plasma chemical vapor deposition. Water plasma lowered the growth temperature down to 450 degrees C, and the grown nanotubes were single-walled without carbonaceous impurities and MWNTs. The preferential growth of pure SWNTs over MWNTs was proven with micro-Raman spectroscopy, high-resolution transmission electron microscopy, and electrical characterization of the grown nanotube networks.     

Nitrogen-doped carbon nanotubes: growth, mechanism and structure

Nitrogen-doped bamboo-structured carbon nanotubes have been successfully grown using a series of cobalt/molybdenum catalysts. The morphology and structure of the nanotubes were analysed by transmission electron microscopy and Raman spectroscopy. The level of nitrogen doping, as determined by X-ray photoelectron spectroscopy, was found to range between 0.5 to 2.5 at.%. The growth of bamboo-structured nanotubes in the presence of nitrogen, in preference to single-walled and multi-walled nanotubes, was due to the greater binding energy of nitrogen for cobalt in the catalyst compared to the binding strength of carbon to cobalt, as determined by density functional theory.     

Application of highly sulfonated single-walled carbon nanotubes: An efficient heterogeneous catalyst for the one-pot synthesis of 14-aryl-14H-dibenzo[a,j]xanthenes under solvent-free conditions

Highly sulfonated single-walled carbon nanotube-catalyzed synthesis of 14-aryl-14H-dibenzo[a,j]xanthenes in excellent yields and very short reaction times. Sulfonated single-walled carbon nanotubes are prepared using a chemical and simple process and it characterized by Scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, Thermal gravimetric analysis (TGA) and acid-base titration. The sulfonated single-walled carbon nanotube was easily separated by simple filtration and was recycled eight consecutive times without any loss in its activity.     

Nanostructured biosensors built by layer-by-layer electrostatic assembly of enzyme-coated single-walled carbon nanotubes and redox polymers

In this study, we describe the construction of glucose biosensors based on an electrostatic layer-by-layer (LBL) technique. Gold electrodes were initially functionalized with negatively charged 11-mercaptoundecanoic acid followed by alternate immersion in solutions of a positively charged redox polymer, poly[(vinylpyridine)Os(bipyridyl)2Cl(2+/3+)], and a negatively charged enzyme, glucose oxidase (GOX), or a GOX solution containing single-walled carbon nanotubes (SWNTs). The LBL assembly of the multilayer films were characterized by UV-vis spectroscopy, ellipsometry, and cyclic voltammetry, while characterization of the single-walled nanotubes was performed with transmission electron microscopy, Raman spectroscopy, thermogravimetric analysis, and X-ray photoelectron spectroscopy. When the GOX solution contained single-walled carbon nanotubes (GOX-SWNTs), the oxidation peak currents during cyclic voltammetry increased 1.4-4.0 times, as compared to films without SWNTs. Similarly the glucose electro-oxidation current also increased (6-17 times) when SWNTs were present. By varying the number of multilayers, the sensitivity of the sensors could be controlled.     

Growth Mechanism of Vertically Aligned Carbon Nanotube Arrays

Vertically aligned multi-walled carbon nanotube arrays grown on quartz substrate are obtained by co-pyrolysis of xylene and ferrocene at 850 oC in a tube furnace. Raman spectroscopy and high resolution transmission electron microscopy measurements show that the single-walled carbon nanotubes are only present on top of vertically aligned multi-walled carbon nanotube arrays. It has been revealed that isolated single-walled carbon nanotubes are only present in those floating catalyst generated materials. It thus suggests that the single-walled carbon nanotubes here are also generated by floating catalyst. Vertically alignedcarbon nanotube arrays on the quartz substrate have shown good orientation and good graphitization. Meanwhile, to investigate the growth mechanism, two bi-layers carbon nan-otube films with di erent thickness have been synthesized and analyzed by Raman spectroscopy. The results show that the two-layer vertically aligned carbon nanotube films grow “bottom-up”. There are distinguished Raman scattering signals for the second layer itself, surface of the first layer, interface between the first and second layer, side wall and bottom surface. It indicates that the obtained carbon nanotubes follow the base-growth mechanism, and the single-walled carbon nanotubes grow from their base at the growth beginning when iron catalyst particles have small size. Those carbon nanotubes with few walls (typically <5 walls) have similar properties, which also agree with the base-growth mechanism.     

Oxidation, deformation, and destruction of carbon nanotubes in aqueous ceric sulfate

A simple wet chemical method involving only ultrasonic processing in dilute ceric sulfate (CS) was used to functionalize carbon nanotubes (CNTs). Unexpectedly, single-walled and multiwalled carbon nanotubes (SWCNTs and MWCNTs) were cut, oxidized, and disintegrated by sonication in 0.1 N CS for 2-5 h. Transmission electron microscopy (TEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction spectroscopy (XRD), Raman scattering, and photoacoustic Fourier transform infrared spectroscopy (FTIR) were used to probe wall damage during the chemical processing. Cyclic voltammetry and impedance spectroscopy were used to evaluate the conductivity of the CS-treated CNTs. This one-step process resulted in the destruction of SWCNTs to produce nonconducting amorphous carbon. MWCNTs were oxidized and converted to graphitic materials and amorphous carbon with retained conductivity.     

High-speed countercurrent chromatography for purification of single-walled carbon nanotubes

A new chromatographic purification of single-walled carbon nanotubes using high-speed countercurrent chromatography is reported. The purification was accomplished on the basis of experiment that dispersed the single-walled carbon nanotubes with sodium dodecyl sulfate, and the result mixture was separated using the two phase system composed of n-butanol/water = 1/1 （v/v）. The sizes of SWNTs separated were observed by scanning electron microscopy. The results demonstrated that the high-speed countercurrent chromatography possessed a good efficency for purification of single-walled carbon nanotubes.     

Spectroscopic investigation of conjugated polymer/single-walled carbon nanotube interactions

Composite materials, based on single-walled carbon nanotubes and a poly(p-phenylene vinylene) derivative, show an interaction between the components capable of solubilising the nanotubes, which has not been otherwise achieved. Here these materials are characterised by electron microscopy, and optical and vibrational spectroscopy. The spectroscopic behaviour of the polymer is seen to be dramatically affected, which is attributed to conformational changes due to the effect of the nanotubes.     

Super-washing does not leave single walled carbon nanotubes iron-free

We demonstrate with transmission electron microscopy and X-ray photoelectron spectroscopy that single-walled carbon nanotubes contain significant amounts of iron in the form of Fe(3)O(4), which even after acid washing, is not removed.     

蒿甲醚在单壁碳纳米管修饰电极上的电催化还原

研制了单壁碳纳米管(SWCNTs)修饰玻碳电极。用交流阻抗谱法(EIS)和扫描电镜(SEM)研究了电极膜性能,应用循环伏安法(CV)、计时库仑法(CC)、计时电流法(CA)研究了蒿甲醚在修饰电极上的电化学行为。结果表明,SWCNTs修饰电极对蒿甲醚的还原有良好的电催化活性,其还原反应为双电子过程,电极反应的扩散系数及速率常数分别为6·67×10-4cm2·s-1及8·54×10-2mol·L-1·s-1。在优化实验条件下,还原峰的峰电位位于-0·85V,其峰电流与蒿甲醚浓度在6·71×10-7~2·45×10-4mol·L-1范围内呈良好线性,检出限达4·02×10-7mol·L-1,相对标准偏差(n=10)为4·2%,可用于蒿甲醚样品的含量测定。     

Direct evidence for root growth of vertically aligned single-walled carbon nanotubes by microwave plasma chemical vapor deposition

The root growth mode of extremely dense and vertically aligned single-walled carbon nanotubes (SWNTs) synthesized by microwave plasma chemical vapor deposition was clarified by a new method, marker growth, which does not require transmission electron microscopy. SWNT layers were grown intermittently on a substrate, and a line between the layers was used as a marker to identify the growth mode. Micro-Raman spectroscopy revealed that the SWNT layers have the same diameter distribution.     

曲克芦丁在羧基化单壁碳纳米管修饰电极上的电化学氧化

研制了羧基化单壁碳纳米管修饰玻碳电极( SWCNTs - COOH/GCE).用交流阻抗谱法(EIS)和扫描电镜( SEM)研究了电极膜性能,应用循环伏安法(CV)考察了曲克芦丁在修饰电极上的电化学行为.结果表明,SWCNTs - COOH修饰电极对曲克芦丁的氧化有良好的电催化活性,其氧化反应为单电子单质子过程,结合恒...     

Characterization of the chemical interaction between single-walled carbon nanotubes and titanium dioxide nanoparticles by thermogravimetric analyses and resonance Raman spectroscopy

Raman spectroscopy is a powerful technique that is used to characterize or observe alterations in the structure or properties of carbon nanotubes and its composites. This method can provide information about electronic changes or quantify them. We used Raman spectroscopy to study the chemical and electronic changes in a composite formed by titanium dioxide nanoparticles and single-walled carbon nanotubes. This composite was characterized by scanning electron microscopy to investigate the morphology and by thermogravimetric analyses to assess the thermal stability of the isolated carbon nanotubes as compared with the nanotubes by titanium dioxide nanoparticles. The Raman results showed that the modification of the nanotubes with the TiO₂ nanoparticles generates a new material with different structure of the nanotubes, resulting in a decrease in defects. The charge transfer from the TiO₂ nanoparticles to the nanotubes alters the electronic properties of both moieties in the hybrid material. The interaction between the nanotubes and nanoparticles decreases the CC bound order of the nanotubes and decreases their thermal stability.     

Layer-by-layer fabrication and characterization of DNA-wrapped single-walled carbon nanotube particles

Carbon nanotubes have been proposed as support materials for numerous applications, including the development of DNA sensors. One of the challenges is the immobilization of DNA or other biological molecules on the sidewall of carbon nanotubes. This paper introduces a new fabrication of DNA-carbon nanotubes particles using the layer-by-layer (LBL) technique on single-walled carbon nanotubes (SWCNTs). Poly(diallyldimethylammonium) (PDDA), a positively charged polyelectrolyte, and DNA as a negatively charged counterpart macromolecule are alternatively deposited on the water-soluble oxidized SWCNTs. Pure DNA/PDDA/SWCNTs particles can be prepared and separated by simple unltracentrifugation. The characterization of DNA/PDDA/SWCNTs particles was carried out by scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-visible spectroscopy, Raman spectroscopy, and thermogravimetric analysis (TGA). An electrode modified by the DNA/PDDA/SWCNTs particles shows a dramatic change of the electrochemical signal in solutions of tris(2,2'-bipyridyl)ruthenium(II) ((Ru(bpy)(3)2+) as a reporting redox probe. A preliminary application of the DNA-modified carbon nanotubes in the development of DNA sensors used in the investigation of DNA damage by nitric oxide is presented.     

A carbon–carbon hybrid – immobilizing carbon nanodots onto carbon nanotubes

The thrust of this work is to integrate small and uniformly sized carbon nanodots (CNDs) with single-walled carbon nanotubes (SWCNT) of different diameters as electron donors and electron acceptors, respectively, and to test their synergetic interactions in terms of optoelectronic devices. CNDs (denoted pCNDs, where p indicates pressure) were prepared by pressure-controlled microwave decomposition of citric acid and urea. pCNDs were immobilized on single-walled carbon nanotubes by wrapping the latter with poly(4-vinylbenzyl trimethylamine) (PVBTA), which features positively charged ammonium groups in the backbone. Negatively charged surface groups on the CNDs lead to attractive electrostatic interactions. Ground state interactions between the CNDs and SWCNTs were confirmed by a full-fledged photophysical investigation based on steady-state and time-resolved techniques. As a complement, charge injection into the SWCNTs upon photoexcitation was investigated by ultra-short time-resolved spectroscopy.     

Application of poly[2-methoxy-5-(2-ethylhexyloxy)-1,4-phenylenevinylene] for splitting of single-walled carbon nanotube bundles in polystyrene/SWCNT composite

Dispersions of single-walled carbon nanotubes (SWCNTs) in organic solutions containing poly[2-methoxy-5-(2-ethylhexyloxy)-1,4-phenylenevinylene] (MEH-PPV) were studied by Raman spectroscopy, UV-vis-NIR spectroscopy, and electron microscopy. This polymer interacts with the nanotube resulting in the appearance of a new red-shifted absorption band in the electronic spectrum. This indicates the formation of a charge-transfer complex between MEH-PPV and SWCNTs. Additives of MEH-PPV make it possible to achieve stable suspensions of nanotubes in styrene. A polystyrene/SWCNT/MEH-PPV composite with a high degree of bundle splitting was obtained by polymerization. It was shown that the luminescence intensity of the nanotubes in the Raman spectrum can serve as a indicator for the estimation of the degree of splitting of SWCNT bundles in the composite.     

Preparation of Hydroxypropyl-β-cyclodextrin Cross-linked Multi-walled Carbon Nanotubes and Their Application in Enantioseparation of Clenbuterol

A method of cross‐linking multi‐walled carbon nanotubes by a nucleophilic substitution of brominated multi‐walled carbon nanotubes using hydroxypropyl‐β‐cyclodextrin anions was studied. The modified multi‐walled carbon nanotube samples were characterized using thermogravimetric analysis, energy‐dispersive X‐ray spectroscopy, transmission electron microscopy, scanning electron microscopy, Raman spectroscopy and Fourier transform infrared spectroscopy. The hydroxypropyl‐β‐cyclodextrin modified multi‐walled carbon nanotubes were used as a chiral stationary phase additive for thin‐layer chromatography to separate clenbuterol enantiomers, and the chiral separation factor was increased.     

Solid-phase microfibers based on polyethylene glycol modified single-walled carbon nanotubes for the determination of chlorinated organic carriers in textiles

Based on polyethylene glycol modified single-walled carbon nanotubes, a novel sol–gel fiber coating was prepared and applied to the headspace microextraction of chlorinated organic carriers (COCs) in textiles by gas chromatography-electron capture detection. The preparation of polyethylene glycol modified single-walled carbon nanotubes and the sol–gel fiber coating process was stated and confirmed by infrared spectra, Raman spectroscopy, and scanning electron microscopy. Several parameters affecting headspace microextraction, including extraction temperature, extraction time, salting-out effect, and desorption time, were optimized by detecting 11 COCs in simulative sweat samples. Compared with the commercial solid-phase microextraction fibers, the sol–gel polyethylene glycol modified single-walled carbon nanotubes fiber showed higher extraction efficiency, better thermal stability, and longer life span. The method detection limits for COCs were in the range from 0.02 to 7.5 ng L⁻¹ (S/N = 3). The linearity of the developed method varied from 0.001 to 50 μg L⁻¹ for all analytes, with coefficients of correlation greater than 0.974. The developed method was successfully applied to the analysis of trace COCs in textiles, the recoveries of the analytes indicated that the developed method was considerably useful for the determination of COCs in ecological textile samples.     

十八醇亲核取代反应修饰溴代多壁碳纳米管

Octadecanol modified multiple-walled carbon nanotubes, with octadecanol covalently bound to the nanotube surface, have been synthesized by bromination of the carbon nanotubes followed by nucleophilic substitution using octadecanol and sodium hydride. Scanning electron microscopy and transmission electron microscopy images show that the morphologies of the nanotubes are largely intact after functionalization. The brominated carbon nanotubes and octadecanol modified carbon nanotubes were characterized using energy-dispersive X-ray spectroscopy, Raman spectroscopy and Fourier transform infrared spectroscopy. The mechanism of nucleophilic substitution was discussed, and it is believed that the reaction occurs with an SN1 mechanism.