Mechanical compliance of photolithographically defined vertically aligned carbon nanotube turf

We describe the micro-mechanical properties of vertically aligned carbon nanotubes (VACNTs) fabricated using a photolithographically patterned iron catalyst prepared using sol–gel techniques. The carbon nanotubes (CNTs) were grown via chemical vapor deposition. The relative mechanical stiffness of the resultant structure was measured using nanoindentation based techniques and is shown to be related to the number of contact sites between tubes. Elastic deformation occurs during compression at large strains, however energy is dissipated during deformation, likely through tube–tube interactions. The effective elastic modulii are depth dependent, due to the compression of pre-buckled geometries. The effective elastic modulii range between 0.03 and 0.08 GPa for a low number of contact sites and 0.1 and 0.3 GPa for a high number of contact sites.     

Quantitative image analysis of polyurethane/carbon nanotube composite micostructures

Polyurethane/carbon nanotube (PUR/CNTs) composites are much more functional than pure polyurethanes. High intensity ultrasonic agitation was applied while preparing a mixture of multiwall carbon nanotubes and a monomer. The monomer/MWNT complexes were used to prepare PUR/CNTs nanocomposites. This paper describes the application of quantitative image analysis to characterise the microstructure of the monomer and segmented polyurethane with carbon nanotubes (CNTs). Stereological parameters chosen for analysis were used to evaluate the CNTs' dispersion in the monomer complex and the degree of matrix phase separation in the nanocomposites examined. The nanoparticles induced changes in the structure of the hard and soft domains in the polyurethane matrix and influenced thermal and mechanical properties of the material. Due to the introduction of the nanotubes in the polyurethane matrix, the physical size and glass transition temperature of hard domains increased while the tensile strength and storage modulus decreased.     

Purity evaluation of carbon nanotube materials by thermogravimetric, TEM, and SEM methods

Raw and purified samples of carbon nanotubes are considered as multicomponent systems with a distribution of carbonaceous, amorphous, multishell graphitic particles and nanotubes, together with the particles of metal compounds from the catalyst. With respect to the carbon nanotube fractions, a distribution of size, defect concentrations, and functionalities needs to be taken into account. In order to address the problem of quantitative evaluation of purity it is necessary to measure the quality and distribution of the carbon nanotubes. In this research conventional and high resolution thermogravimetry are applied to quantify different fractions of carbonaceous and metallic materials in raw and moderately purified single walled and multiwalled carbon nanotubes. For each oxidized fraction, defined by careful line shape analysis of the derivative thermogravimetric curves (DTG), the temperature of maximum rate of oxidation, the temperature range for this oxidation, related to the degree of homogeneity, and the amount of associated material is specified. The attribution of carbonaceous materials to each fraction in the distribution was based on SEM and TEM measurements and the literature. The MWNT purified sample with 1.6 wt% metal oxide was investigated by high resolution thermogravimetry (HRTG). The quantitative assessment for the carbonaceous fractions was 25 wt% of amorphous and high defect carbonaceous materials including nanotubes, 54 wt% MWNT and 20 wt% multishell graphitic particles. A qualitative evaluation of these fractions was obtained from the SEM and TEM images and supports these results. The accuracy of the values, taking into account other measurements performed on the same batch of material, should be more sensible than +/-4 wt%.     

Preparation and characterization of polystyrene-multiwalled carbon nanotube composite fibers by electrospinning

Electrospinning is a simple technique to prepare polymer fibers in nanometer diameters using very high electrostatic fields. These nanofibers are useful in many applications since the surface area to volume ratio in these fibers is very high. Here we have prepared nanofibers of composites of Polystyrene (PS) with different concentrations (0.05% to 2% w/w) of multi-walled carbon nanotubes (MWCNT) by electrospinning. The fibers are characterized by SEM, TEM, Raman spectra, and TGA. The room temperature electrical conductivity of single fibers of these composites are measured and found to show dramatic improvement in the conductivity due to the addition of MWCNT to the polymer matrix compared to the pure PS.     

Electrochemical characterization of parylene-embedded carbon nanotube nanoelectrode arrays

A novel parylene-embedded carbon nanotube nanoelectrode array is presented for use as an electrochemical detector working electrode material. The fabrication process is compatible with standard microfluidic and other MEMS processing without requiring chemical mechanical polishing. Electrochemical studies of the nanoelectrodes showed that they perform comparably to platinum. Electrochemical pretreatment for short periods of time was found to further improve performance as measured by cathodic and anodic peak separation of K(3)Fe(CN)(6). A lower detection limit below 0.1?μM was measured and with further fabrication improvements detection limits between 100?pM and 10?nM are possible. This makes the nanoelectrode arrays particularly suitable for trace electrochemical analysis.     

Carbon nanotube purification: preparation and characterization of carbon nanotube paste electrodes

Paste electrodes have been constructed using single-wall carbon nanotubes mixed with mineral oil. The electrochemical behavior of such electrodes prepared with different percentages of carbon nanotubes has been compared with that of graphite paste electrodes and evaluated with respect to the electrochemistry of ferricyanide with cyclic voltammetry. Carbon nanotubes were purified by a treatment with concentrated nitric acid, then oxidized in air. In addition, electrochemical pretreatments were carried out to increase the selectivity of carbon nanotube electrodes. Performances of carbon nanotube paste and carbon paste electrodes were evaluated by studying such parameters as current peak, deltaEp, anodic and cathodic current ratio, and charge density toward several different electroactive molecules. Data interpretation based on the carbon nanotubes and carbon surface area is presented. Carbon nanotube paste and carbon paste electrodes were tested as H2O2 and NADH probes, and several analytical parameters were evaluated. The oxidative behavior of dopamine was examined at these electrodes. The two-electron oxidation of dopamine to dopaminequinone showed an excellent reversibility in cyclic voltammetry that was significantly better than that observed at carbon paste electrodes.     

低温等离子体增强化学气相沉积技术制备碳纳米管

由于等离子体在低温下具有高活性的特点,等离子体增强化学气相沉积(PECVD)技术可显著降低薄膜沉积的温度范围.通常条件下,高质量碳纳米管的生长要求800℃以上的基片温度,若能使该温度降到400℃以下,则对许多应用非常有利,如可以在玻璃基片上沉积碳纳米管场发射电极.目前,碳纳米管基纳电子器件的研制这一课题备受关注,如果能实现低温原位制备碳纳米管,则可能将纳电子器件与传统的微电子加工工艺结合并实现超大容量的超大规模集成电路.本文主要介绍近年来生长碳纳米管所采用的各种等离子体化学气相沉积技术,讨论影响碳纳米管生长特性的几个关键因素.     

Efficient fabrication of carbon nanotube micro tip arrays by tailoring cross-stacked carbon nanotube sheets

Carbon nanotube (CNT) micro tip arrays with hairpin structures on patterned silicon wafers were efficiently fabricated by tailoring the cross-stacked CNT sheet with laser. A blade-like structure was formed at the laser-cut edges of the CNT sheet. CNT field emitters, pulled out from the end of the hairpin by an adhesive tape, can provide 150 μA intrinsic emission currents with low beam noise. The nice field emission is ascribed to the Joule-heating-induced desorption of the emitter surface by the hairpin structure, the high temperature annealing effect, and the surface morphology. The CNT emitters with hairpin structures will greatly promote the applications of CNTs in vacuum electronic devices and hold the promises to be used as the hot tips for thermochemical nanolithography. More CNT-based structures and devices can be fabricated on a large scale by this versatile method.     

碳纳米管/聚乙烯咪唑纳米复合材料的制备与表征

采用化学改性手段制备了一类新型的碳纳米管／聚乙烯咪唑(CNTs／PVI)纳米复合材料。并通过红外光谱、扫描电镜、透射电镜和X射线衍射等手段表征CNTs／PVI产物。有机杂环聚合物引入碳纳米管材料体系以后,会显著改善碳纳米管在有机溶剂中的分散均匀性和可加工性,并将碳纳米管具有的优异力学、热稳定性能和杂环聚合物具有的优良溶解性等结合起来,得到一种新型的综合性能优异的光电功能材料。     

Synthesis and characterization of multiwalled carbon nanotube/FeCo nanocomposites

Multiwalled carbon nanotube/FeCo nanocomposites were produced by Catalytic Chemical Vapour Deposition using highly porous FeCo-SiO2 aerogels with different loadings and dimensions of FeCo nanoparticles as catalysts. Multiwalled carbon nanotubes with average number of walls depending on the size of the catalyst nanoparticles were obtained. Inside the nanotubes spherical or elliptical FeCo nanoparticles are retained, and the magnetic properties of the resulting nanocomposites were characterized in detail.     

On the mechanical characterization of carbon nanotube reinforced epoxy adhesives

In this work, the mechanical properties of carbon nanotube reinforced epoxy adhesives are investigated experimentally. The investigations are intended to characterize the physical and mechanical properties of nano-reinforced structural epoxy adhesives and to further highlight some of the complex phenomena associated with these materials. We describe the dispersion methodology used to disperse the carbon nanotubes into the considered adhesive and provide details pertaining to adherent surface preparation, bondline thickness control and adhesive curing conditions. Furthermore, the following tests are described: (i) dogbone tensile testing, (ii) tensile bond testing, (iii) double lap shear and (iv) double cantilever beam fracture toughness testing. The experimental observations indicate a critical carbon nanotube concentration in the vicinity of 1.5 wt% that results in the largest improvements in the measured properties. At concentrations exceeding this critical value, the properties begin to degrade, in some cases, to levels below that of the pure epoxy. Advanced electron microscopy techniques and rheological assessments indicate that this is mainly due to the agglomeration of the carbon nanotubes at higher concentrations as a result of increased resin viscosity and the consequent resistance to dispersion.     

Preparation and characterization of carbon nanotube/polyetherimide nanocomposite films

Multi-walled carbon nanotube (MWCNT)/polyetherimide (PEI) nanocomposite films have been prepared by casting and imidization. A homogeneous dispersion of MWCNTs throughout the PEI matrix is observed by scanning electron microscopy of fracture surfaces, which shows not only a fine dispersion of MWCNTs but also strong interfacial adhesion with the matrix, as evidenced by the presence of many broken but strongly embedded carbon nanotubes (CNTs) in the matrix and by the absence of debonding of CNTs from the matrix. Differential scanning calorimetry and dynamic mechanical analysis show that the glass transition temperature of PEI increases by about 10 °C by the addition of 1 wt% MWCNTs. Mechanical testing shows that for the addition of 1 wt% MWCNTs, the elastic moduli of the nanocomposites are significantly improved by about 250% while the tensile strength is comparable to that of the matrix. This improvement is due to the strong interfacial interaction between the MWCNTs and the PEI matrix which favors stress transfer from the polymer to the CNTs.     

Non-destructive characterization of structural hierarchy within aligned carbon nanotube assemblies

Understanding and controlling the hierarchical self-assembly of carbon nanotubes (CNTs) is vital for designing materials such as transparent conductors, chemical sensors, high-performance composites, and microelectronic interconnects. In particular, many applications require high-density CNT assemblies that cannot currently be made directly by low-density CNT growth, and therefore require post-processing by methods such as elastocapillary densification. We characterize the hierarchical structure of pristine and densified vertically aligned multi-wall CNT forests, by combining small-angle and ultra-small-angle x-ray scattering (USAXS) techniques. This enables the nondestructive measurement of both the individual CNT diameter and CNT bundle diameter within CNT forests, which are otherwise quantified only by delicate and often destructive microscopy techniques. Our measurements show that multi-wall CNT forests grown by chemical vapor deposition consist of isolated and bundled CNTs, with an average bundle diameter of 16 nm. After capillary densification of the CNT forest, USAXS reveals bundles with a diameter >4 μm, in addition to the small bundles observed in the as-grown forests. Combining these characterization methods with new CNT processing methods could enable the engineering of macro-scale CNT assemblies that exhibit significantly improved bulk properties.     

Preparation and characterization of carbon nanotube reinforced silicon nitride composites

Multiwall carbon nanotube (MWNT) reinforced silicon nitride ceramics matrix composites have been prepared. The hot isostatic press (HIP)-sintering method was used for composite processing. Bending strength and elastic modulus of MWNT-silicon nitride composites showed a considerable improvement compared to matrices with added carbon fiber, carbon black or graphite. However, the silicon nitride samples without any carbon addition, because of higher densities present an even higher value. In the case of carbon fibers addition, a deterioration during sintering has been observed. The increasing pressure and sintering time resulted in carbon nanotube free structures.     

Efficient spectrofluorimetric analysis of single-walled carbon nanotube samples

A new method and instrumentation are described for rapid compositional analysis of single-walled carbon nanotube (SWCNT) samples. The customized optical system uses multiple fixed-wavelength lasers to excite NIR fluorescence from SWCNTs individualized in aqueous suspensions. The emission spectra are efficiently captured by a NIR spectrometer with InGaAs multichannel detector and then analyzed by a computer program that consults a database of SWCNT spectral parameters. The identities and relative abundances of semiconducting SWCNTs species are quickly deduced and displayed in graphs and tables. Results are found to be consistent with those based on manual interpretation of full excitation-emission scans from a conventional spectrofluorometer. The new instrument also measures absorption spectra using a broadband lamp and multichannel spectrometers, allowing samples to be automatically characterized by their emission efficiencies. The system provides rapid data acquisition and is sensitive enough to detect the fluorescence of a few picograms of SWCNTs in ~50 μL sample volumes.     

Resonance Raman spectroscopy characterization of single-wall carbon nanotube separation by their metallicity and diameter

Several techniques were recently reported for the bulk separation of metallic (M) and semiconducting (S) single wall carbon nanotubes (SWNTs), using optical absorption and resonance Raman spectroscopy (RRS) as a proof of the separation. In the present work, we develop a method for the quantitative evaluation of the M to S separation ratio, and also for the SWNT diameter selectivity of the separation process, based on RRS. The relative changes in the integrated intensities of the radial-breathing mode (RBM) features, with respect to the starting material, yield the diameter probability distribution functions for M and S SWNTs in the separated fractions, accounting for the different resonance conditions of individual SWNTs, while the diameter distribution of the starting material is obtained following the fitting procedure developed by Kuzmany and coworkers. Features other than the RBM are generally less effective for characterization of the separation process for SWNTs.     

Formation and microstructural characterization of coaxial carbon cylinders consisting of aligned carbon nanotube stacks

The macroscopic coaxial carbon cylinders (dia. approximately 0.5 cm with varying lengths approximately 2-5 cm) consisting of aligned carbon nanotube (CNT) stacks have been prepared by spray pyrolysis of benzene-ferrocene solution in argon atmosphere at approximately 850 degrees C-900 degrees C temperature. The coaxial carbon cylinders of CNT stacks have been formed directly inside the quartz tube. We attempted to prepare superimposed multi carbon cylinder configurations, each consisting of ordered and aligned CNTs stacked over each other. For this, we have terminated the spray of precursor after run of about 25 minutes, for a short interval (approximately 5 min), and then the solution was sprayed again over the already deposited hot CNT stack. Gross structural characterization of CNTs was done through X-ray diffraction technique (XRD). Microstructural characterizations of as prepared coaxial carbon cylinders with CNT stacks were done by scanning electron microscopic (SEM) techniques. SEM studies show that the CNTs are well aligned along the periphery of the cross section of coaxial carbon cylinder, each consisting of CNTs of the type described in the above. Comparisons have been made between the present macroscopic coaxial carbon cylinders with CNT stacks studied earlier by several other workers. Plausible explanation for the synthesis of CNT stacks will be put forward.     

Synthesis and characterization of nano-scale alumina on single walled carbon nanotube

In this study, nano-scale crystalline alumina was synthesized on single walled carbon nanotube by sol-gel method for using as a sorbent for solid phase extraction of trace metals. The characterization of the synthesized nanocomposite material was performed by scanning electron microscope, transmission electron microscope and X-ray diffractometer methods. It was proved that the obtained composite material was mainly nano-scale Al₂O₃, and partly Mg₂Al₂O₄ and Zn₂Al₂O₄ on single walled carbon nanotube. In addition, the specific surface area of the material was determined and found as 165 m²/g. The adsorption capacity of the nanomaterial was also determined for cadmium(II) ions and found as 2.18 mg/g at pH 8.     

Microfabrication and characterization of spray-coated single-wall carbon nanotube film strain gauges

We present the design, fabrication, and characterization results of single-wall carbon nanotube (SWCNT) film strain gauges for potential applications as highly sensitive strain, weight, or pressure sensors on the macro-scale. A batch microfabrication process was developed for practical device construction and packaging using spray-coated SWCNTs and a conventional semiconductor process. The prototype was characterized using a commercial metal foil gauge with tensile and compressive testing on a binocular load cell. Our test results demonstrated that the proposed SWCNT film gauges have a linear relationship between resistance changes and externally applied strain. The gauge factor ranged from 7.0 to 16.4 for four different micro-grid configurations, indicating that the maximum strain sensitivity of the prototype was approximately eight times greater than that of commercial gauges.     

碳纳米管/导电聚苯胺纳米复合纤维的合成与表征

为实现碳纳米管在树脂内形成一体化导电网络,从而制备出透明导电性能最优的有机透明导电涂层,必须把导电性的碳纳米管纤维在树脂内有效地组装成一体化导电结构网络。本文报道运用在树脂内可以自组装的导电苯胺来实现碳纳米管纤维自组装的方法．合成出了导电聚苯胺纳米薄膜均匀包覆的碳纳米管/导电聚苯胺纳米复合纤维．并运用透射电镜、傅立叶红外光谱以及四探针法表面电阻测试仪对合成出的具有精细微观结构的纳米复合纤维进行了表征．发现合成出了理想的碳纳米管/导电聚苯胺纳米复合纤维,并且其导电性较碳纳米管和导电聚苯胺自身都有大幅度的提高。这种特殊结构的纳米复合纤维的制备为组装高性能的聚合物基透明导电涂层奠定了坚实基础,而且这种自组装方法为各种纳米纤维的组装提供了可能。