Estimation of agglomerate size of multi-walled carbon nanotubes in fluidized beds

The objective of this study was to determine hydrodynamic characteristics of multi-walled carbon nanotubes (MWCNTs) agglomerates and examine their sizes. The bed collapsing process of MWCNTs agglomerates was found to be closer to that of Geldart group C particles than group A particles. Median diameters of MWCNTs agglomerates determined by sedimentation method at initial superficial gas velocity of 0.120 and 0.190 m/s were 157 and 221 μm, respectively. The size of these MWCNTs agglomerates in fluidization state was measured by image analysis using a high speed camera. Median diameters of these MWCNTs agglomerates in freeboard were increased from 138 to 189 μm as superficial gas velocity was increased from 0.088 to 0.190 m/s at static bed height of 0.16 m. Median diameter and size distribution determined by sedimentation method fitted well with those measured using image analysis. Results were reasonable at superficial gas velocity up to 0.190 m/s.     

Voltammetric determination of norepinephrine in the presence of acetaminophen using a novel ionic liquid/multiwall carbon nanotubes paste electrode

A novel multiwall carbon nanotubes (MWCNTs) modified carbon ionic liquid electrode (CILE) was fabricated and used to investigate the electrochemical behavior of norepinephrine (NP). MWCNTs/CILE was prepared by mixing hydrophilic ionic liquid, 1-methyl-3-butylimidazolium bromide (MBIDZBr), with graphite powder, MWCNTs, and liquid paraffin. The fabricated MWCNTs/CILE showed great electrocatalytic ability to the oxidation of NE. The electron transfer coefficient, diffusion coefficient, and charge transfer resistant (R_ct) of NE at the modified electrode were calculated. Differential pulse voltammetry of NE at the modified electrode exhibited two linear dynamic ranges with slopes of 0.0841 and 0.0231 μA/μM in the concentration ranges of 0.3 to 30.0 μM and 30.0 to 450.0 μM, respectively. The detection limit (3σ) of 0.09 μM NP was achieved. This modified electrode exhibited a good ability for well separated oxidation peaks of NE and acetaminophen (AC) in a buffer solution, pH 7.0. The proposed sensor was successfully applied for the determination of NE in human urine, pharmaceutical, and serum samples.     

Magnetic properties and transmission electron microscopy studies of Ni nanoparticles encapsulated in carbon nanocages and carbon nanotubes

Three types of carbon nanomaterials, including bamboo-shaped carbon nanotubes with Ni encapsulated and hollow and Ni catalytic particles filled carbon nanocages, have been prepared by methane catalytic decomposition at a relatively low temperature. Transmission electron microscopy observations showed that fascinating fullerene-like Ni–C (graphitic) core–shell nanostructures predominated. Detailed examination of high-resolution transmission electron microscopy showed that the walls of bamboo-shaped carbon nanotubes with quasi-cone catalytic particles encapsulated consisted of oblique graphene planes with respect to the tube axis. The Ni particles encapsulated in the carbon nanocages were larger than that encapsulated in carbon nanotubes, but the diameters of the cores of hollow carbon nanocages were less than that of Ni particles encapsulated in carbon nanotubes, suggesting that the sizes of catalyst particles played an important role during carbon nanomaterial growth. The magnetic properties of the carbon nanomaterials were measured, which showed relatively large coercive force (H_c = 138.4 O_e) and good ferromagnetism (M_r/M_s = 0.325).     

Some of the physical and mechanical properties of cement composites manufactured from carbon nanotubes and bagasse fiber

The objective of this investigation was to evaluate physical and mechanical properties of experimental cement type panels made from multi-wall carbon nanotubes (MWCNTs) and bagasse fiber. Three levels of MWCNTs, namely 0.5 wt.%, 1 wt.% and 1.5 wt.% were mixed with 10 wt.% and 20 wt.% of bagasse fiber in rotary type mixer. Thickness swelling, water absorption, bending characteristics and impact strength of the samples were evaluated. Based on the findings in this work the water absorption and thickness swelling of the nanocomposites decreased with increasing amount of the multi-wall carbon nanotubes content in the panels from 0.5% to 1.5%. On the other hand flexural modulus and impact strength of the panels were enhanced with increased percentage of carbon nanotubes. Panels having 0.5% MWCNTs exhibited the highest impact strength. Overall dimensional stability and strength properties of the samples were adversely influenced with increased amount bagasse fiber in the samples. It appears that using lower percentage of bagasse fiber or application of heat or chemical treatment to the raw material should be considered to improve negative influence of bagasse fiber on properties of the panels.     

Thermal and mechanical properties of phenolic-based composites reinforced by carbon fibres and multiwall carbon nanotubes

The thermal, mechanical and ablation properties of carbon fibre/phenolic composites filled with multiwall carbon nanotubes (MWCNTs) were investigated. Carbon fibre/phenolic/MWCNTs were prepared using different weight percentage of MWCNTs by compression moulding. The samples were characterized by scanning electron microscopy (SEM), flexural tests, thermal gravimetric analysis and oxyacetylene torch tests. The thermal stability and flexural properties of the nanocomposites increased by increasing MWCNTs content (wt% ⩽1), but they decreased when the content of MWCNTs was 2 wt%. The linear and mass ablation rates of the nanocomposites after modified with 1 wt% MWCNTs decreased by about 80% and 52%, respectively. To investigate the material post-test microstructure, a morphological characterization was carried out using SEM. It was shown that the presence of MWCNTs in the composite led to the formation of a strong network char layer without any cracks or opening.     

Characterization of carbon nanotubes decorated with NiFe2O4 magnetic nanoparticles as a novel electrochemical sensor: Application for highly selective determination of sotalol using voltammetry

A magnetic nano‐composite of multiwall carbon nanotube, decorated with NiFe₂O₄ nanoparticles, was synthesized with citrate sol–gel method. The multiwall carbon nanotubes decorated with NiFe₂O₄ nanoparticles (NiFe₂O₄–MWCNTs) were characterized with different methods such as Fourier transform infrared spectroscopy (FT‐IR), transmission electron microscopy (TEM), atomic force microscopy (AFM), vibrating sample magnetometer (VSM), cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS). The new nano-composite acts as a suitable electrocatalyst for the oxidation of sotalol at a potential of 500 mV at the surface of the modified electrode. Linear sweep voltammetry exhibited two wide linear dynamic ranges of 0.5–1000 μmol L^? 1 sotalol with a detection limit of 0.09 μmol L^? 1. The modified electrode was used as a novel electrochemical sensor for the determination of sotalol in real samples such as pharmaceutical, patient and safe human urine.     

Strain sensing in polymer/carbon nanotube composites by electrical resistance measurement

In this work multiwall carbon nanotubes (MWCNTs) dispersed in a polymer matrix have been used for strain sensing of the resulting nanocomposite under tensile loading. This was achieved by measuring the relative electrical resistance change (ΔR/R₀) in conductive polyvinylidenefluoride (PVDF)/MWCNTs nanocomposites prepared by melt-mixing with varying filler content from 0.5 wt.% to 8 wt.%. Two main parameters were systematically studied. The PVDF/MWCNTs mixing procedure that results in a successful MWCNTs dispersion, and the effect of MWCNTs content on material’s sensing behaviour. The samples were subjected to tensile loading and the longitudinal strain was monitored together with the longitudinal electrical resistance. The results showed that MWCNTs dispersed in insulating PVDF matrix have the potential to be used as a sensitive network to monitor the strain levels in polymer/carbon nanotube nanocomposites as the deformation level of each sample was being reflected by the resistance changes.     

Microstructural characteristics and mechanical properties of carbon nanotube reinforced aluminum alloy composites produced by ball milling

The influence of milling time on the structure, morphology and thermal stability of multi-walled carbon nanotubes (MWCNTs) reinforced EN AW6082 aluminum alloy powders has been studied. After structural and microstructural characterization of the mechanically milled powders micro- and nano-hardness of the composite powder particles were evaluated. The morphological and X-ray diffraction studies on the milled powders revealed that the carbon nanotubes (CNTs) were uniformly distributed and embedded within the aluminum matrix. No reaction products were detected even after long milling up to 50 h. Nanotubes became shorter in length as they fractured under the impact and shearing action during the milling process. A high hardness of about 436 ± 52 HV is achieved for the milled powders, due to the addition of MWCNTs, after milling for 50 h. The increased elastic modulus and nanohardness can be attributed to the finer grain size evolved during high energy ball milling and to the uniform distribution of hard CNTs in the Al-alloy matrix. The hardness values of the composite as well as the matrix alloy compares well with that predicted by the Hall–Petch relationship.     

Determination of Pb2+ ions by a modified carbon paste electrode based on multi-walled carbon nanotubes (MWCNTs) and nanosilica

A novel carbon paste ion selective electrode for determination of trace amount of lead was prepared. Multi-walled carbon nanotubes (MWCNTs) and nanosilica were used for improvement of a lead carbon paste sensor response. MWCNTs have a good conductivity which helps the transduction of the signal in carbon paste electrode. The electrode composition of 20 wt% paraffin oil, 57% graphite powder, 15% ionophore (thiram), 5% MWCNTs, and 3% nanosilica showed the stable potential response to Pb²⁺ ions with the Nernstian slope of 29.8 (±0.2) mV decade^?1 over a wide linear concentration range of 10^?7–10^?2 mol L^?1. The electrode has fast response time, and long term stability (more than 2 months). The proposed electrode was used to determine the concentration of lead ions in waste water and black tea samples.     

Fabrication of a selective mercury sensor based on the adsorption of cold vapor of mercury on carbon nanotubes: Determination of mercury in industrial wastewater

A new sensor for the determination of mercury at μg ml^?1 levels is proposed based on the adsorption of mercury vapor on single-walled carbon nanotubes (SWCNTs). The changes in the impedance of SWCNTs were monitored upon adsorption of mercury vapor. The adsorption behaviour of mercury on SWCNTs was compared with that on multi-walled carbon nanotubes (MWCNTs) and carbon nanofibers (CNFs). Cold vapor of mercury was generated at 65 °C using Sn(II) solution as a reducing agent. The limit of detection was 0.64 μg ml^?1 for Hg(II) species. The calibration curve for Hg(II) was linear from 1.0 to 30.0 μg ml^?1. The relative standard deviation (RSD) of eight replicate analyses of 15 μg ml^?1 of Hg(II) was 2.7%. The results showed no interfering effects from many foreign species and hydride forming elements. The system was successfully applied to the determination of the mercury content of different types of wastewater samples.     

An investigation of electrochemical behavior of nanofluids containing MWCNT on the corrosion rate of carbon steel

In this research, the corrosion rate of carbon steel in nanosuspensions containing multi-walled carbon nanotubes (MWCNT) is investigated by using potentiodynamic polarization measurements. It was observed that functionalized MWCNTs prevent carbon steel corrosion to some extent in comparison with the distillated water, but by adding MWCNTs to the SDS and SDBS water solution, the corrosion current increased. On the other hand, after adding acid-based commercial inhibitor to the functionalized sample, in the range of 12–100 ppm, polarization measurements indicated an increase in the corrosion rate of carbon steel from 0.538 to 4.26 mpy. This increase is believed to be due to the enhanced mass transfer of species to and from the metal, as well as the partial destruction of functional groups on CNTs by the protective layer adsorbed (such as SDS) on the carbon steel surface. Also by using a basic CSI inhibitor (nitrite based), corrosion rate decreased to 0.499 mpy.     

Amperometric choline biosensors based on multi-wall carbon nanotubes and layer-by-layer assembly of multilayer films composed of Poly(diallyldimethylammonium chloride) and choline oxidase

A layer-by-layer deposition technique combined with Multi-wall carbon nanotubes (MWCNTs) was employed for fabricating choline sensors. The terminals and side-walls were linked with oxygen-containing groups when MWCNTs were treated with concentrated acid mixtures. A film of MWCNTs was initially prepared on the platinum electrode surface. Based on the electrostatic interaction between positively charged polyallylamine (PAA) and negatively charged MWCNTs and poly(vinyl sulfate) (PVS), a polymer film of (PVS/PAA)₃ was alternately adsorbed on the modified electrode continuously to be used as a permselective layer. Then poly(diallyldimethylammonium) (PDDA) and choline oxidase(ChOx) multilayer films were assembled layer-by-layer on the pretreated electrode, so an amplified biosensor toward choline was constructed. The choline sensor showed a linear response range of 5 × 10^? 7 to 1 × 10^? 4 M with a detection limit of 2 × 10^? 7 M estimated at a signal-to-noise ratio of 3, and a sensitivity of 12.53 μA/mM with a response time of 7.6 s in the presence of MWCNTs. Moreover, it exhibited excellent reproducibility, long-term stability as well as good suppression of interference. This protocol could be used to immobilize other enzymes for biosensor fabrication.     

Controllable synthesis of multi-layer graphene flakes and multi-wall carbon nanotubes from pyrolyzing biodegradable poly(butylene succinate) composites

This work reports a simple method to synthesize multi-layer graphene flakes (MLGFs) and multi-wall carbon nanotubes (MWCNTs) from pyrolyzing biodegradable poly(butylene succinate) (―[OC(CH₂)₂COO(CH₂)₄O]_n―) composites. The obtained carbon nanomaterials were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD). The SEM and TEM results indicated that the morphology of the carbon nanomaterials was significantly influenced by the catalyst precusors used. When MnO₂ was used as the catalyst precusor, MLGFs with the thickness between 1.4 and 4 nm were produced. However, when Ni₂O₃ was used, MWCNTs with the diameter of 18–28 nm were obtained. The XRD patterns demonstrated that MnO and Ni, in situ formed from MnO₂ and Ni₂O₃, were the active sites for the formation of MLGFs and MWCNTs respectively. On the basis of the results, a possible formation mechanism of MLGFs and MWCNTs was proposed.     

Synthesis of multi-walled carbon nanotubes using Co–Fe–Mo/Al2O3 catalytic powders in a fluidized bed reactor

The effects of the metal loading (30–70 wt.%), metal molar ratio (Co/Fe, 1–5) and mass ratio of citric acid to the catalyst (0–0.6) on the productivity and mean diameter of the multi-walled carbon nanotubes (MWCNTs) in a gas–solid fluidized bed reactor (with an inner diameter of 0.056 m and a height of 1.0 m) were determined. Liquefied petroleum gas (LPG) was used as the carbon source. X-ray diffraction (XRD) was used to characterize the catalysts synthesized using a combustion method. MWCNTs synthesized in the fluidized bed reactor were characterized by field emission scanning electron microscopy (FE-SEM) to observe their morphologies and measure their diameters. Productivity was increased by increasing both the metal loading and the mass ratio of citric acid to the catalyst. A high productivity, up to 2000%, was obtained. The catalyst transition metal particle grain size decreased in the range of 8–17 nm with an increasing citric acid mass ratio to the catalyst and the mean diameter of the MWCNTs decreased with increasing the metal molar ratio, however the correlation between the grain size in the catalyst and the mean diameter of MWCNTs remains unclear.     

Reduction of thermal residual stresses of laminated polymer composites by addition of carbon nanotubes

This paper studies the effects of multi-walled carbon nanotubes (MWCNTs) on the thermal residual stresses in polymeric fibrous composites. Reinforced ML-506 epoxy nanocomposites with different amounts of homogeneously dispersed MWCNTs (0.1 wt.%, 0.5 wt.% and 1 wt.%) were fabricated using the sonication technique. Thermo-mechanical analysis and tensile tests of the specimens were carried out to characterize the thermal and mechanical properties of MWCNTs/epoxy composites. Due to the negative thermal expansion and high modulus of MWCNTs, addition of MWCNTs resulted in a great reduction of the coefficient of thermal expansion (CTE) of epoxy. The MWCNTs also moderately increased the Young’s modulus of the epoxy. Then, the effects of adding MWCNTs on micro and macro-residual stresses in carbon fiber (CF)/epoxy laminated composites were investigated using the energy method and the classical lamination theory (CLT), respectively. The results indicated that the addition of low amounts of MWCNTs leads to a considerable reduction in thermal residual stress components in both micro and macro levels.     

Methoxypolyethylene glycol functionalized carbon nanotube composites with high permittivity and low dielectric loss

High relative permittivity and low dielectric loss were simultaneously achieved in the percolative nanocomposites with methoxypolyethylene glycol (mPEG) modified multi-walled carbon nanotubes (MWCNTs). The dense mPEG layer with a thickness of approximately 1.7 nm was continuously coated on the surface of MWCNTs. MWCNTs exhibited excellent dispersibility after being functionalized by mPEG (mPEG@MWCNTs), the mPEG@MWCNTs/ethanol suspension was still turbid even when the suspension was deposited for two months. A high permittivity of 69.7 and a low dielectric loss of 0.042 were simultaneously achieved in the poly(vinylidene fluoride-co-hexafluoropropylene) (P(VDF-HFP)) nanocomposite with 4.02 vol% mPEG@MWCNTs at 1 kHz. The improved dielectric properties in the nanocomposite is mainly ascribed to the following reasons: (i) the increased microcapacitors formed by MWCNTs and insulated dielectric composite; (ii) the enhanced interfacial polarization due to the homogeneous dispersion of mPEG@MWCNTs in the nanocomposites and tight adhesion between mPEG@MWCNTs and P(VDF-HFP) matrix.     

Effect of amino-functionalization on the interfacial adhesion of multi-walled carbon nanotubes/epoxy nanocomposites

Two types of multi-walled carbon nanotubes (MWCNTs) functionalized with different amino-organics, dicyanodiamide and phenylbiguanide, respectively, were achieved in this paper. The physico-chemical properties of MWCNTs before and after amino group modification were characterized by thermogravimetric analysis (TGA), Raman spectroscopy and inverse gas chromatography (IGC). The results showed that amino-functionalization changed evidently the surface properties of MWCNTs, such as the dispersive surface energy (decreased from 122.95 mJ/m² to 18.65 mJ/m² and 25.69 mJ/m², respectively) and specific surface energy (decreased from 8.84 mJ/m² to 0.56 mJ/m² and 4.60 mJ/m², respectively) for two functionalized MWCNTs. And then, the interfacial adhesion states of the functionalized MWCNTs/epoxy nanocomposites were investigated using scanning electron microscope (SEM) and dynamic mechanical analysis (DMA). The results also indicated that the dispersion of MWCNTs in epoxy resin and the interfacial adhesion of MWCNTs/epoxy nanocomposites were both strongly dependent on the surface physico-chemical properties of functionalized MWCNTs, and the effect of MWCNTs functionalized by phenylbiguanide with slightly higher polarity was better.     

Synthesis of zinc oxide particles coated multiwalled carbon nanotubes: Dielectric properties,electromagnetic interference shielding and microwave absorption

Zinc oxide (ZnO) nanoparticles were coated on the surfaces of multiwalled carbon nanotubes (MWCNTs). High resolution transmission electron microscopy images show that the wurtzite ZnO immobilized on the MWCNTs is single-crystalline with a preferential [0 0 0 2] growth direction. A capacitor was generated by the interface of ZnO and MWCNTs, and a resistor–capacitor model could well describe the relationships between the structure and the dielectric properties, electromagnetic interference shielding and microwave-absorption of the composites in the frequency range of 2–18 GHz. The network built by ZnO-immobilized MWCNTs could contribute to the improvement of electrical properties. Resonant peaks associated with the capacitor formed by the interface were observed in the microwave absorption spectra, which suggest that reflection–loss peaks greatly broadens the absorption bandwidth.     

Upgrading of low-grade gold ore samples for improved particle characterisation using Micro-CT and SEM/EDX

There is a considerable challenge in accurate characterisation of gold (Au) particles in low-grade plant ore mineral samples. This is particularly true for automated mineralogical tools such as X-ray micro-computed tomography (Micro-CT) and scanning electron microscopy (SEM), where the need for statistically meaningful numbers of particles requires many sections to be analysed. Whiles the Vertical Gas Stream (VGS) elutriator is suitable for coarse particle upgrading (i.e. >38 μm), the performance is poor for finer particles (i.e. <38 μm). Consequently, the system has been modified to Vertical Water Stream (VWS) elutriator using higher density fluid (i.e. water) to enable analysis of Au particles below 38 μm. In this work, the VGS system was used to upgrade Au particles in the ?53 + 38 μm size fraction (in rougher concentrate, rougher tailings, regrind mill discharge and regrind cyclone underflow) and the VWS system was used to upgrade Au particles in the ?38 μm size fraction of the regrind mill discharge sample. The VWS elutriator was calibrated using galena (specific gravity, S.G. of 7.58) and quartz (S.G. of 2.65) particles of <38 μm size as model minerals. From the calibration tests, partition curves as a function of particle size were generated. Using these measurements, theoretical partition curves for Au (S.G. of 19.3) have been calculated. The VWS concentrate was characterised using Micro-CT and compared with SEM coupled with energy dispersive X-ray (EDX) analysis of ?53 + 38 μm ore size fraction of the VGS concentrate of the four sample streams. The Micro-CT analysis of VWS Au concentrate showed that sufficient particles (Au) can be upgraded. SEM/EDX results indicate that regrind does not affect changes in free Au particle morphology, aspect ratio and frequency of shearing damage in the ?53 + 38 μm size fraction. Cyclone classification of the regrind mill discharge in the ?53 + 38 μm size fraction appears to perform surface cleaning by exposing obscuring silver (Ag) surfaces on Au particles in the mill discharge sample.     

Microstructure and mechanical property of multi-walled carbon nanotubes reinforced aluminum matrix composites fabricated by friction stir processing

Aluminum matrix composites reinforced by different contents of multi-walled carbon nanotubes (MWCNTs) were fabricated by friction stir processing (FSP). The microstructure of nano-composites and the interface between aluminum matrix and MWCNTs were examined using optical microscopy (OM) and transmission electron microscopy (TEM). It was indicated that MWCNTs were well dispersed in the aluminum matrix throughout the FSP. Tensile tests and microhardness measurement showed that, with the increase of MWCNT content, the tensile strength and microhardness of MWCNTs/Al composites gradually increased, but on the contrary, the elongation decreased. The maximum ultimate tensile strength reached up to 190.2 MPa when 6 vol.% MWCNTs were added, and this value was two times more of that of aluminum matrix. Appearances and fracture surface micrographs of failed composite samples indicated that the composites become more and more brittle with the increase of the MWCNT content.