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1.  Delivery of small interfering RNAs in human cervical cancer cells by polyethylenimine-functionalized carbon nanotubes 
Nanoscale Research Letters  2013;8(1):267.
Carbon nanotubes are capable of penetrating the cell membrane and are widely considered as potential carriers for gene or drug delivery. Because the C-C and C=C bonds in carbon nanotubes are nonpolar, functionalization is required for carbon nanotubes to interact with genes or drugs as well as to improve their biocompatibility. In this study, polyethylenimine (PEI)-functionalized single-wall (PEI-NH-SWNTs) and multiwall carbon nanotubes (PEI-NH-MWNTs) were produced by direct amination method. PEI functionalization increased the positive charge on the surface of SWNTs and MWNTs, allowing carbon nanotubes to interact electrostatically with the negatively charged small interfering RNAs (siRNAs) and to serve as nonviral gene delivery reagents. PEI-NH-MWNTs and PEI-NH-SWNTs had a better solubility in water than pristine carbon nanotubes, and further removal of large aggregates by centrifugation produced a stable suspension of reduced particle size and improved homogeneity and dispersity. The amount of grafted PEI estimated by thermogravimetric analysis was 5.08% (w/w) and 5.28% (w/w) for PEI-NH-SWNTs and PEI-NH-MWNTs, respectively. For the assessment of cytotoxicity, various concentrations of PEI-NH-SWNTs and PEI-NH-MWNTs were incubated with human cervical cancer cells, HeLa-S3, for 48 h. PEI-NH-SWNTs and PEI-NH-MWNTs induced cell deaths in a dose-dependent manner but were less cytotoxic compared to pure PEI. As determined by electrophoretic mobility shift assay, siRNAs directed against glyceraldehyde-3-phosphate dehydrogenase (siGAPDH) were completely associated with PEI-NH-SWNTs or PEI-NH-MWNTs at a PEI-NH-SWNT/siGAPDH or PEI-NH-MWNT/siGAPDH mass ratio of 80:1 or 160:1, respectively. Furthermore, PEI-NH-SWNTs and PEI-NH-MWNTs successfully delivered siGAPDH into HeLa-S3 cells at PEI-NH-SWNT/siGAPDH and PEI-NH-MWNT/siGAPDH mass ratios of 1:1 to 20:1, resulting in suppression of the mRNA level of GAPDH to an extent similar to that of DharmaFECT, a common transfection reagent for siRNAs. Our results indicate that the PEI-NH-SWNTs and PEI-NH-MWNTs produced in this study are capable of delivering siRNAs into HeLa-S3 cells to suppress gene expression and may therefore be considered as novel nonviral gene delivery reagents.
doi:10.1186/1556-276X-8-267
PMCID: PMC3683344  PMID: 23742156
SWNTs; MWNTs; PEI; Small interfering RNA; Gene delivery
2.  Enhancing performance of ZnO dye-sensitized solar cells by incorporation of multiwalled carbon nanotubes 
Nanoscale Research Letters  2012;7(1):166.
A low-temperature, direct blending procedure was used to prepare composite films consisting of zinc oxide [ZnO] nanoparticles and multiwalled carbon nanotubes [MWNTs]. The mesoporous ZnO/MWNT films were fabricated into the working electrodes of dye-sensitized solar cells [DSSCs]. The pristine MWNTs were modified by an air oxidation or a mixed acid oxidation treatment before use. The mixed acid treatment resulted in the disentanglement of MWNTs and facilitated the dispersion of MWNTs in the ZnO matrix. The effects of surface property and loading of MWNTs on DSSC performance were investigated. The performance of DSSCs was found to depend greatly on the type and the amount of MWNTs incorporated. At a loading of 0.01 wt%, the acid-treated MWNTs were able to increase the power conversion efficiency of fabricated cells from 2.11% (without MWNTs) to 2.70%.
doi:10.1186/1556-276X-7-166
PMCID: PMC3320520  PMID: 22390565
ZnO; nanoparticle; multiwalled carbon nanotube; composite film; dye-sensitized solar cells; conversion efficiency
3.  In situ Polymerization of Multi-Walled Carbon Nanotube/Nylon-6 Nanocomposites and Their Electrospun Nanofibers 
Nanoscale Research Letters  2008;4(1):39-46.
Multiwalled carbon nanotube/nylon-6 nanocomposites (MWNT/nylon-6) were prepared by in situ polymerization, whereby functionalized MWNTs (F-MWNTs) and pristine MWNTs (P-MWNTs) were used as reinforcing materials. The F-MWNTs were functionalized by Friedel-Crafts acylation, which introduced aromatic amine (COC6H4-NH2) groups onto the side wall. Scanning electron microscopy (SEM) images obtained from the fractured surfaces of the nanocomposites showed that the F-MWNTs in the nylon-6 matrix were well dispersed as compared to those of the P-MWNTs. Both nanocomposites could be electrospun into nanofibers in which the MWNTs were embedded and oriented along the nanofiber axis, as confirmed by transmission electron microscopy. The specific strength and modulus of the MWNTs-reinforced nanofibers increased as compared to those of the neat nylon-6 nanofibers. The crystal structure of the nylon-6 in the MWNT/nylon-6 nanofibers was mostly γ-phase, although that of the MWNT/nylon-6 films, which were prepared by hot-pressing the pellets between two aluminum plates and then quenching them in icy water, was mostly α-phase, indicating that the shear force during electrospinning might favor the γ-phase, similarly to the conventional fiber spinning.
doi:10.1007/s11671-008-9199-0
PMCID: PMC2893824  PMID: 20596470
In situ polymerization; Nylon-6; Nanofibers; Carbon nanotube; Nanocomposite
4.  In situ Polymerization of Multi-Walled Carbon Nanotube/Nylon-6 Nanocomposites and Their Electrospun Nanofibers 
Nanoscale Research Letters  2008;4(1):39-46.
Multiwalled carbon nanotube/nylon-6 nanocomposites (MWNT/nylon-6) were prepared by in situ polymerization, whereby functionalized MWNTs (F-MWNTs) and pristine MWNTs (P-MWNTs) were used as reinforcing materials. The F-MWNTs were functionalized by Friedel-Crafts acylation, which introduced aromatic amine (COC6H4-NH2) groups onto the side wall. Scanning electron microscopy (SEM) images obtained from the fractured surfaces of the nanocomposites showed that the F-MWNTs in the nylon-6 matrix were well dispersed as compared to those of the P-MWNTs. Both nanocomposites could be electrospun into nanofibers in which the MWNTs were embedded and oriented along the nanofiber axis, as confirmed by transmission electron microscopy. The specific strength and modulus of the MWNTs-reinforced nanofibers increased as compared to those of the neat nylon-6 nanofibers. The crystal structure of the nylon-6 in the MWNT/nylon-6 nanofibers was mostly γ-phase, although that of the MWNT/nylon-6 films, which were prepared by hot-pressing the pellets between two aluminum plates and then quenching them in icy water, was mostly α-phase, indicating that the shear force during electrospinning might favor the γ-phase, similarly to the conventional fiber spinning.
doi:10.1007/s11671-008-9199-0
PMCID: PMC2893824  PMID: 20596470
In situ polymerization; Nylon-6; Nanofibers; Carbon nanotube; Nanocomposite
5.  Characterization of Multiwalled Carbon Nanotube-Reinforced Hydroxyapatite Composites Consolidated by Spark Plasma Sintering 
BioMed Research International  2014;2014:768254.
Pure HA and 1, 3, 5, and 10 vol% multiwalled carbon nanotube- (MWNT-) reinforced hydroxyapatite (HA) were consolidated using a spark plasma sintering (SPS) technique. The relative density of pure HA increased with increasing sintering temperature, but that of the MWNT/HA composite reached almost full density at 900°C, and then decreased with further increases in sintering temperature. The relative density of the MWNT/HA composites increased with increasing MWNT content due to the excellent thermal conductivity of MWNTs. The grain size of MWNT/HA composites decreased with increasing MWNT content and increased with increasing sintering temperature. Pull-out toughening of the MWNTs of the MWNT/HA composites was observed in the fractured surface, which can be used to predict the improvement of the mechanical properties. On the other hand, the existence of undispersed or agglomerate MWNTs in the MWNT/HA composites accompanied large pores. The formation of large pores increased with increasing sintering temperature and MWNT content. The addition of MWNT in HA increased the hardness and fracture toughness by approximately 3~4 times, despite the presence of large pores produced by un-dispersed MWNTs. This provides strong evidence as to why the MWNTs are good candidates as reinforcements for strengthening the ceramic matrix. The MWNT/HA composites did not decompose during SPS sintering. The MWNT-reinforced HA composites were non-toxic and showed a good cell affinity and morphology in vitro for 1 day.
doi:10.1155/2014/768254
PMCID: PMC3960548  PMID: 24724100
6.  Free Energetics of Carbon Nanotube Association in Pure and Aqueous Ionic Solutions 
The journal of physical chemistry. B  2012;116(28):8154-8168.
Carbon nanotubes are a promising platform across a broad spectrum of applications ranging from separations technology, drug delivery, to bio(electronic) sensors. Proper dispersion of carbon nanotube materials is important to retaining the electronic properties of nanotubes. Experimentally it has been shown that salts can regulate the dispersing properties of CNTs in aqueous system with surfactants (J. Am. Chem. Soc., 2009, 131:1144–1153); details of the physico-chemical mechanisms underlying such effects continue to be explored. We address the effects of inorganic monovalent salts (NaCl and NaI) on dispersion stability of carbon nanotubes. We perform all-atom molecular dynamics simulations using non-polarizable interaction models to compute the potential of mean force between two (10,10) single-walled carbon nanotubes (SWNTs) in the presence of NaCl/NaI and compare to the potential of mean force between SWNTs in pure water. Addition of salts enhances stability of the contact state between two SWNT’s on the order of 4 kcal/mole. The ion-specific spatial distribution of different halide anions gives rise to starkly different contributions to the free energy stability of nanotubes in the contact state. Iodide anion directly stabilizes the contact state to a much greater extent than chloride anion. The enhanced stability arises from the locally repulsive forces imposed on nanotubes by the surface-segregated iodide anion. Within the timescale of our simulations, both NaI and NaCl solutions stabilize the contact state by equivalent amounts. The marginally higher stability for contact state in salt solutions recapitulates results for small hydrophobic solutes in NaCl solutions (Athawale et al, J. Phys. Chem. B., 112, 5661. 2008) as well as single walled carbon nanotubes in NaCl and CaCl2 aqueous solutions.
doi:10.1021/jp3025717
PMCID: PMC3562760  PMID: 22780909
single-walled nanotubes; hydrophobic effect; specific-ion effects; molecular dynamics simulation
7.  Exploring the Chemical Sensitivity of a Carbon Nanotube/Green Tea Composite 
ACS nano  2010;4(11):6854-6862.
Single-walled carbon nanotubes (SWNTs) possess unique electronic and physical properties, which make them very attractive for a wide range of applications. In particular, SWNTs and their composites have shown a great potential for chemical and biological sensing. Green tea, or more specifically its main antioxidant component, epigallocatechin gallate (EGCG), has been found to disperse SWNTs in water. However, the chemical sensitivity of this SWNT/green tea (SWNT/EGCG) composite remained unexplored. With EGCG present, this SWNT composite should have strong antioxidant properties and thus respond to reactive oxygen species (ROS). Here we report on fabrication and characterization of SWNT/EGCG thin films and the measurement of their relative conductance as a function of H2O2 concentrations. We further investigated the sensing mechanism by Fourier-transform infrared (FTIR) spectroscopy and field-effect transistor measurements (FET). We propose here that the response to H2O2 arises from the oxidation of EGCG in the composite. These findings suggest that SWNT/green tea composite has a great potential for developing simple resistivity-based sensors.
doi:10.1021/nn100988t
PMCID: PMC3026703  PMID: 21043457
resistivity sensors; ROS; hydrogen peroxide; relative humidity
8.  Pt-TiO2/MWCNTs Hybrid Composites for Monitoring Low Hydrogen Concentrations in Air 
Sensors (Basel, Switzerland)  2012;12(9):12361-12373.
Hydrogen is a valuable fuel for the next energy scenario. Unfortunately, hydrogen is highly flammable at concentrations higher than 4% in air. This aspect makes the monitoring of H2 leaks an essential issue for safety reasons, especially in the transportation field. In this paper, nanocomposites based on Pt-doped TiO2/multiwalled carbon nanotubes (MWCNTs) have been introduced as sensitive materials for H2 at low temperatures. Pt-TiO2/MWNTs nanocomposites with different composition have been prepared by a simple wet chemical procedure and their morphological, microstructural and electrical properties were investigated. Resistive thick-film devices have been fabricated printing the hybrid nanocomposites on alumina substrates provided with Pt interdigitated electrodes. Electrical tests in air have shown that embedding MWCNTs in the TiO2 matrix modify markedly the electrical conductivity, providing a means to decrease the resistance of the sensing layer. Pt acts as a catalytic additive. Pt-TiO2/MWNTs-based sensors were found to be sensitive to hydrogen at concentrations between 0.5 and 3% in air, satisfying the requisites for practical applications in hydrogen leak detection devices.
doi:10.3390/s120912361
PMCID: PMC3478844
hydrogen sensor; TiO2; MWCNTs; hybrid nanocomposites
9.  Repair of Abdominal Wall Defects In Vitro and In Vivo Using VEGF Sustained-Release Multi-Walled Carbon Nanotubes (MWNT) Composite Scaffolds 
PLoS ONE  2013;8(5):e64358.
Objective
Porcine acellular dermal matrices (ADM) have been widely used in experimental and clinical research for abdominal wall repair. Compared to porcine small intestinal submucosa (SIS), the effect of these matrices on the regenerative capacity of blood vessels is still not ideal. Multi-walled carbon nanotubes (MWNTs) can more effectively transport VEGF to cells or tissues because of their large specific surface area and interior cavity. In this study, we explored the safety and efficacy of implanted VEGF-loaded MWNT composite scaffolds in vitro and vivo to repair abdominal wall defects.
Materials and Methods
VEGF-loaded MWNTs were prepared by a modified plasma polymerization treatment. Four composite scaffolds were evaluated for cytotoxicity, proliferation, and release dynamics. We created 3 cm×4 cm abdominal wall defects in 43 Sprague-Dawley rats. After implantation times of 2, 4, 8, and 12 weeks, the scaffolds and the surrounding tissues were collected and examined by gross inspection, biomechanical testing, and histological examination.
Results
A 5–10 nm poly(lactic-co-glycolic acid) (PLGA) film was evenly distributed on MWNTs. The 3% MWNT composite group showed lower cytotoxicity and appropriate release performance, and it was thus tested in vivo. In rats with the 3% composite implanted, host cells were prevented from migrating to the ADM at 2 weeks, vascularization was established more rapidly at 12 weeks, and the values for both the maximum load and the elastic modulus were significantly lower than in the ADM-alone group (p<0.01). Histological staining revealed that the MWNT was still not completely eliminated 12 weeks after implantation.
Conclusion
MWNTs were able to carry VEGF to cells or tissues, and the 3% MWNT composite material showed lower cytotoxicity and had an appropriate release performance, which prompted faster vascularization of the ADM than other scaffolds. Nevertheless, the MWNTs induced harmful effects that should be carefully considered in biomedical studies.
doi:10.1371/journal.pone.0064358
PMCID: PMC3661462  PMID: 23717603
10.  Enhancements of thermal conductivities with Cu, CuO, and carbon nanotube nanofluids and application of MWNT/water nanofluid on a water chiller system 
Nanoscale Research Letters  2011;6(1):297.
In this study, enhancements of thermal conductivities of ethylene glycol, water, and synthetic engine oil in the presence of copper (Cu), copper oxide (CuO), and multi-walled carbon nanotube (MWNT) are investigated using both physical mixing method (two-step method) and chemical reduction method (one-step method). The chemical reduction method is, however, used only for nanofluid containing Cu nanoparticle in water. The thermal conductivities of the nanofluids are measured by a modified transient hot wire method. Experimental results show that nanofluids with low concentration of Cu, CuO, or carbon nanotube (CNT) have considerably higher thermal conductivity than identical base liquids. For CuO-ethylene glycol suspensions at 5 vol.%, MWNT-ethylene glycol at 1 vol.%, MWNT-water at 1.5 vol.%, and MWNT-synthetic engine oil at 2 vol.%, thermal conductivity is enhanced by 22.4, 12.4, 17, and 30%, respectively. For Cu-water at 0.1 vol.%, thermal conductivity is increased by 23.8%. The thermal conductivity improvement for CuO and CNT nanofluids is approximately linear with the volume fraction. On the other hand, a strong dependence of thermal conductivity on the measured time is observed for Cu-water nanofluid. The system performance of a 10-RT water chiller (air conditioner) subject to MWNT/water nanofluid is experimentally investigated. The system is tested at the standard water chiller rating condition in the range of the flow rate from 60 to 140 L/min. In spite of the static measurement of thermal conductivity of nanofluid shows only 1.3% increase at room temperature relative to the base fluid at volume fraction of 0.001 (0.1 vol.%), it is observed that a 4.2% increase of cooling capacity and a small decrease of power consumption about 0.8% occur for the nanofluid system at a flow rate of 100 L/min. This result clearly indicates that the enhancement of cooling capacity is not just related to thermal conductivity alone. Dynamic effect, such as nanoparticle dispersion may effectively augment the system performance. It is also found that the dynamic dispersion is comparatively effective at lower flow rate regime, e.g., transition or laminar flow and becomes less effective at higher flow rate regime. Test results show that the coefficient of performance of the water chiller is increased by 5.15% relative to that without nanofluid.
doi:10.1186/1556-276X-6-297
PMCID: PMC3211363  PMID: 21711787
11.  Ecological Uptake and Depuration of Carbon Nanotubes by Lumbriculus variegatus 
Environmental Health Perspectives  2008;116(4):496-500.
Background
Carbon nanotubes represent a class of nanomaterials having broad application potentials and documented cellular uptake and ecotoxicological effects that raise the possibility that they may bioaccumulate in living organisms.
Objectives
Radioactively labeled nanotubes were synthesized using a novel methane chemical vapor deposition procedure. Single-walled carbon nanotubes (SWNTs), multiwalled carbon nanotubes (MWNTs), and pyrene were spiked to sediment samples, and the respective uptake and depuration of these nanotubes and pyrene were assessed by the oligochaete, Lumbriculus variegatus.
Results
14C-labeled carbon nanotubes were developed for these experiments to overcome significant previous limitations for quantifying nanotube materials in environmental and biological media. Biota-sediment accumulation factors for SWNTs and MWNTs were observed to be almost an order of magnitude lower than those for pyrene, a four-ringed polycyclic aromatic hydrocarbon (PAH). The depuration behaviors of the oligochaete suggested that the nanotubes detected in these organisms were associated with sediments remaining in the organism guts and not absorbed into cellular tissues as was the pyrene. The results suggest that, unlike PAHs, purified carbon nanotubes do not readily absorb into organism tissues.
doi:10.1289/ehp.10883
PMCID: PMC2290976  PMID: 18414633
bioaccumulation; carbon nanotubes; ecotoxicology; environmental risks; fullerenes; Lumbriculus variegatus; MWNT; nanomaterials; nanotechnology; SWNT
12.  Carbon Nanotube Nanoreservior for Controlled Release of Anti-inflammatory Dexamethasone 
Biomaterials  2011;32(26):6316-6323.
On demand release of anti-inflammatory drug or neurotropic factors have great promise for maintaining a stable chronic neural interface. Here we report the development of an electrically controlled drug release system based on conducting polymer and carbon nanotubes. Drug delivery research using carbon nanotubes (CNTs) has taken advantage of the ability of CNTs to load large amounts of drug molecules on their outer surface. However, the utility of the inner cavity of CNTs, which can increase the drug loading capacity, has not yet been explored. In this paper, the use of multi-wall CNTs as nanoreserviors for drug loading and controlled release is demonstrated. The CNTs are pretreated with acid sonication to open their ends and make their outer and inner surfaces more hydrophilic. When dispersed and sonicated in a solution containing the anti-inflammatory drug dexamethasone, experiments show that the pretreated CNTs are filled with the drug solution. To prevent the unwanted release of the drug, the open ends of the drug-filled CNTs are then sealed with polypyrrole (PPy) films formed through electropolymerization. The prepared electrode coating significantly reduced the electrode impedance, which is desired for neural recording and stimulation. More importantly, the coating can effectively store drug molecules and release the bioactive drug in a controlled manner using electrical stimulation. The dexamethasone released from the PPy/CNT film was able to reduce lipopolysaccharide induced microglia activation to the same degree as the added dexamethasone.
doi:10.1016/j.biomaterials.2011.05.020
PMCID: PMC3387429  PMID: 21636128
13.  Transparent Conductors from Carbon Nanotubes LBL-Assembled with Polymer Dopant with π-π Electron Transfer 
Single-walled carbon nanotube (SWNT) and other carbon-based coatings are being considered as replacements for indium tin oxide (ITO). The problems of transparent conductors (TCs) coatings from SWNT and similar materials include poor mechanical properties, high roughness, low temperature resilience, and fast loss of conductivity. The simultaneous realization of these desirable characteristics can be achieved using high structural control of layer-by-layer (LBL) deposition, which is demonstrated by the assembly of hydroethyl cellulose (HOCS) and sulfonated polyetheretherketone (SPEEK)-SWNTs. A new type of SWNT doping based on electron transfer from valence bands of nanotubes to unoccupied levels of SPEEK through π-π interactions was identified for this system. It leads to a conductivity of 1.1×105 S/m at 66wt% loadings of SWNT. This is better than other polymer/SWNT composites and translates into surface conductivity of 920 ohms/sq and transmittance of 86.7% at 550nm. The prepared LBL films also revealed unusually high temperature resilience up to 500°C, and low roughness of 3.5 nm (ITO glass - 2.4 nm). Tensile modulus, ultimate strength, and toughness of such coatings are 13±2 GPa, 366±35 MPa and 8±3 kJ/m3, respectively, and exceed corresponding parameters of all similar TCs. The cumulative figure of merit, ΠTC, which included the critical failure strain relevant for flexible electronics, was ΠTC = 0.022 and should be compared to ΠTC = 0.006 for commercial ITO. Further optimization is possible using stratified nanoscale coatings and improved doping from the macromolecular LBL components.
doi:10.1021/ja111687t
PMCID: PMC3136082  PMID: 21524068
carbon nanotube; sulfonated polyetherether ketone; hydroxyethyl cellulose; transparent conductors; layer-by-layer; nanocomposites; conductivity; mechanical strength; helical wrapping; doping
14.  Fabrication of a Microbial Biosensor Based on QD-MWNT Supports by a One-Step Radiation Reaction and Detection of Phenolic Compounds in Red Wines 
Sensors (Basel, Switzerland)  2011;11(2):2001-2012.
An Acaligense sp.-immobilized biosensor was fabricated based on QD-MWNT composites as an electron transfer mediator and a microbe immobilization support by a one-step radiation reaction and used for sensing phenolic compounds in commercial red wines. First, a quantum dot-modified multi-wall carbon nanotube (QD-MWNT) composite was prepared in the presence of MWNT by a one-step radiation reaction in an aqueous solution at room temperature. The successful preparation of the QD-MWNT composite was confirmed by XPS, TEM, and elemental analysis. Second, the microbial biosensor was fabricated by immobilization of Acaligense sp. on the surface of the composite thin film of a glassy carbon (GC) electrode, which was prepared by a hand casting method with a mixture of the previously obtained composite and Nafion solution. The sensing ranges of the microbial biosensor based on CdS-MWNT and Cu2S-MWNT supports were 0.5–5.0 mM and 0.7–10 mM for phenol in a phosphate buffer solution, respectively. Total concentration of phenolic compounds contained in commercial red wines was also determined using the prepared microbial immobilized biosensor.
doi:10.3390/s110202001
PMCID: PMC3274030  PMID: 22319395
microbial biosensor; quantum dots; one-step radiation reaction; electron transfer supports; phenolic compounds; red wines
15.  Development of n-type cobaltocene-encapsulated carbon nanotubes with remarkable thermoelectric property 
Scientific Reports  2015;5:7951.
Direct conversion from heat to electricity is one of the important technologies for a sustainable society since large quantities of energy are wasted as heat. We report the development of a single-walled carbon nanotube (SWNT)-based high conversion efficiency, air-stable and flexible thermoelectric material. We prepared cobaltocene-encapsulated SWNTs (denoted CoCp2@SWNTs) and revealed that the material showed a negative-type (n-type) semiconducting behaviour (Seebeck coefficient: −41.8 μV K−1 at 320 K). The CoCp2@SWNT film was found to show a high electrical conductivity (43,200 S m−1 at 320 K) and large power factor (75.4 μW m−1 K−2) and the performance was remarkably stable under atmospheric conditions over a wide range of temperatures. The thermoelectric figure of merit (ZT) value of the CoCp2@SWNT film (0.157 at 320 K) was highest among the reported n-type organic thermoelectric materials due to the large power factor and low thermal conductivity (0.15 W m−1 K−1). These characteristics of the n-type CoCp2@SWNTs allowed us to fabricate a p-n type thermoelectric device by combination with an empty SWNT-based p-type film. The fabricated device exhibited a highly efficient power generation close to the calculated values even without any air-protective coating due to the high stability of the SWNT-based materials under atmospheric conditions.
doi:10.1038/srep07951
PMCID: PMC4302313  PMID: 25608478
16.  Supercapacitance from Cellulose and Carbon Nanotube Nanocomposite Fibers 
ACS Applied Materials & Interfaces  2013;5(20):9983-9990.
Multiwalled carbon nanotube (MWNT)/cellulose composite nanofibers have been prepared by electrospinning a MWNT/cellulose acetate blend solution followed by deacetylation. These composite nanofibers were then used as precursors for carbon nanofibers (CNFs). The effect of nanotubes on the stabilization of the precursor and microstructure of the resultant CNFs were investigated using thermogravimetric analysis, transmission electron microscopy and Raman spectroscopy. It is demonstrated that the incorporated MWNTs reduce the activation energy of the oxidative stabilization of cellulose nanofibers from ∼230 to ∼180 kJ mol–1. They also increase the crystallite size, structural order, and electrical conductivity of the activated CNFs (ACNFs). The surface area of the ACNFs increased upon addition of nanotubes which protrude from the fiber leading to a rougher surface. The ACNFs were used as the electrodes of a supercapacitor. The electrochemical capacitance of the ACNF derived from pure cellulose nanofibers is demonstrated to be 105 F g–1 at a current density of 10 A g–1, which increases to 145 F g–1 upon the addition of 6% of MWNTs.
doi:10.1021/am403622v
PMCID: PMC3807724  PMID: 24070254
cellulose; supercapacitor; nanocomposites
17.  Compressive Strength, Chloride Permeability, and Freeze-Thaw Resistance of MWNT Concretes under Different Chemical Treatments 
The Scientific World Journal  2014;2014:572102.
This study investigated compressive strength, chloride penetration, and freeze-thaw resistance of multiwalled carbon nanotube (MWNT) concrete. More than 100 cylindrical specimens were used to assess test variables during sensitivity observations, including water-cement ratios (0.75, 0.5, and 0.4) and exposure to chemical agents (including gum arabic, propanol, ethanol, sodium polyacrylate, methylcellulose, sodium dodecyl sulfate, and silane). To determine the adequate sonication time for MWNT dispersal in water, the compressive strengths of MWNT concrete cylinders were measured after sonication times ranging from 2 to 24 minutes. The results demonstrated that the addition of MWNT can increase the compressive strength of concrete by up to 108%. However, without chemical treatment, MWNT concretes tend to have poor freeze-thaw resistance. Among the different chemical treatments, MWNT concrete treated with sodium polyacrylate has the best compressive strength, chloride resistance, and freeze-thaw durability.
doi:10.1155/2014/572102
PMCID: PMC4130312  PMID: 25140336
18.  Synthesis of Carbon Nanotube (CNT) Composite Membranes 
Membranes  2010;1(1):37-47.
Carbon nanotubes are attractive approach for designing of new membranes for advanced molecular separation because of their unique transport properties and ability to mimic biological protein channels. In this work the synthetic approach for fabrication of carbon nanotubes (CNTs) composite membranes is presented. The method is based on growth of multi walled carbon nanotubes (MWCNT) using chemical vapour deposition (CVD) on the template of nanoporous alumina (PA) membranes. The influence of experimental conditions including carbon precursor, temperature, deposition time, and PA template on CNT growth process and quality of fabricated membranes was investigated. The synthesis of CNT/PA composites with controllable nanotube dimensions such as diameters (30–150 nm), and thickness (5–100 μm), was demonstrated. The chemical composition and morphological characteristics of fabricated CNT/PA composite membranes were investigated by various characterisation techniques including scanning electron microscopy (SEM), energy-dispersive x-ray spectroscopy (EDXS), high resolution transmission electron microscopy (HRTEM) and x-ray diffraction (XRD). Transport properties of prepared membranes were explored by diffusion of dye (Rose Bengal) used as model of hydrophilic transport molecule.
doi:10.3390/membranes1010037
PMCID: PMC4056580  PMID: 24957494
carbon nanotubes; nanoporous alumina membranes; electrochemical anodization; catalyst free carbon precursor; transport properties
19.  Characterization of Electrosynthesized Conjugated Polymer-Carbon Nanotube Composite: Optical Nonlinearity and Electrical Property 
The effects of multi-walled carbon nanotube (MWNT) concentration on the structural, optical and electrical properties of conjugated polymer-carbon nanotube composite are discussed. Multi-walled carbon nanotube-polypyrrole nanocomposites were synthesized by electrochemical polymerization of monomers in the presence of different amounts of MWNTs using sodium dodecylbenzensulfonate (SDBS) as surfactant at room temperature and normal pressure. Field emission scanning electron microscopy (FESEM) indicates that the polymer is wrapped around the nanotubes. Measurement of the nonlinear refractive indices (n2) and the nonlinear absorption (β) of the samples with different MWNT concentrations measurements were performed by a single Z-scan method using continuous wave (CW) laser beam excitation wavelength of λ = 532 nm. The results show that both nonlinear optical parameters increased with increasing the concentration of MWNTs. The third order nonlinear susceptibilities were also calculated and found to follow the same trend as n2 and β. In addition, the conductivity of the composite film was found to increase rapidly with the increase in the MWNT concentration.
doi:10.3390/ijms13010918
PMCID: PMC3269728  PMID: 22312294
conducting polymers; carbon nanotubes; optical properties; electrical characterization
20.  Cytotoxicity Screening of Single-Walled Carbon Nanotubes: Detection and Removal of Cytotoxic Contaminants from Carboxylated Carbon Nanotubes 
Molecular pharmaceutics  2011;8(4):1351-1361.
This study compares the cytotoxicity to cultured mammalian cells of nine different single-walled carbon nanotube (SWNT) products synthesized by a variety of methods and obtained from a cross section of vendors. A standard procedure involving sonication and centrifugation in buffered bovine serum albumin was developed to disperse all the SWNTs in a biocompatible solution to facilitate comparisons. The effect of the SWNTs on the proliferative ability of a standard cell line was then assessed. Of the nine different SWNT materials tested, only two were significantly toxic, and both were functionalized by carboxylation from different vendors. This was unexpected because carboxylation makes SWNTs more water soluble, which would presumably correlate with better biocompatibility. However, additional purification work demonstrated that the toxic material in the carboxylated SWNT preparations could be separated from the SWNTs by filtration. The filtrate that contained the toxic activity also contained abundant small carbon fragments that had Raman signatures characteristic of amorphous carbon species, suggesting a correlation between toxicity and oxidized carbon fragments. The removal of a toxic contaminant associated with carboxylated SWNTs is important in the development of carboxylated SWNTs for pharmacological applications.
doi:10.1021/mp2001439
PMCID: PMC3148312  PMID: 21688794
carbon nanotubes; nanotoxicology; cytotoxicity; amorphous carbon; carboxylation
21.  Selective Deposition and Alignment of Single-Walled Carbon Nanotubes Assisted by Dielectrophoresis: From Thin Films to Individual Nanotubes 
Nanoscale Research Letters  2010;5(6):1072-1078.
Dielectrophoresis has been used in the controlled deposition of single-walled carbon nanotubes (SWNTs) with the focus on the alignment of nanotube thin films and their applications in the last decade. In this paper, we extend the research from the selective deposition of SWNT thin films to the alignment of small nanotube bundles and individual nanotubes. Electrodes with “teeth”-like patterns are fabricated to study the influence of the electrode width on the deposition and alignment of SWNTs. The entire fabrication process is compatible with optical lithography-based techniques. Therefore, the fabrication cost is low, and the resulting devices are inexpensive. A series of SWNT solutions is prepared with concentrations ranging from 0.0125 to 0.2 mg/ml. The alignment of SWNT thin films, small bundles, and individual nanotubes is achieved under the optimized experimental conditions. The electrical properties of these samples are characterized; the linear current–voltage plots prove that the aligned SWNTs are mainly metallic nanotubes. The microscopy inspection of the samples demonstrates that the alignment of small nanotube bundles and individual nanotubes can only be achieved using narrow electrodes and low-concentration solutions. Our investigation shows that it is possible to deposit a controlled amount of SWNTs in desirable locations using dielectrophoresis.
doi:10.1007/s11671-010-9604-3
PMCID: PMC2894206  PMID: 20672073
Single-walled carbon nanotubes (SWNT); Dielectrophoresis (DEP); Thin film; Nanotube bundle; Individual nanotube; Deposition
22.  Selective Deposition and Alignment of Single-Walled Carbon Nanotubes Assisted by Dielectrophoresis: From Thin Films to Individual Nanotubes 
Nanoscale Research Letters  2010;5(6):1072-1078.
Dielectrophoresis has been used in the controlled deposition of single-walled carbon nanotubes (SWNTs) with the focus on the alignment of nanotube thin films and their applications in the last decade. In this paper, we extend the research from the selective deposition of SWNT thin films to the alignment of small nanotube bundles and individual nanotubes. Electrodes with “teeth”-like patterns are fabricated to study the influence of the electrode width on the deposition and alignment of SWNTs. The entire fabrication process is compatible with optical lithography-based techniques. Therefore, the fabrication cost is low, and the resulting devices are inexpensive. A series of SWNT solutions is prepared with concentrations ranging from 0.0125 to 0.2 mg/ml. The alignment of SWNT thin films, small bundles, and individual nanotubes is achieved under the optimized experimental conditions. The electrical properties of these samples are characterized; the linear current–voltage plots prove that the aligned SWNTs are mainly metallic nanotubes. The microscopy inspection of the samples demonstrates that the alignment of small nanotube bundles and individual nanotubes can only be achieved using narrow electrodes and low-concentration solutions. Our investigation shows that it is possible to deposit a controlled amount of SWNTs in desirable locations using dielectrophoresis.
doi:10.1007/s11671-010-9604-3
PMCID: PMC2894206  PMID: 20672073
Single-walled carbon nanotubes (SWNT); Dielectrophoresis (DEP); Thin film; Nanotube bundle; Individual nanotube; Deposition
23.  Single-walled carbon nanotube interactions with HeLa cells 
This work concerns exposing cultured human epithelial-like HeLa cells to single-walled carbon nanotubes (SWNTs) dispersed in cell culture media supplemented with serum. First, the as-received CoMoCAT SWNT-containing powder was characterized using scanning electron microscopy and thermal gravimetric analyses. Characterizations of the purified dispersions, termed DM-SWNTs, involved atomic force microscopy, inductively coupled plasma – mass spectrometry, and absorption and Raman spectroscopies. Confocal microRaman spectroscopy was used to demonstrate that DM-SWNTs were taken up by HeLa cells in a time- and temperature-dependent fashion. Transmission electron microscopy revealed SWNT-like material in intracellular vacuoles. The morphologies and growth rates of HeLa cells exposed to DM-SWNTs were statistically similar to control cells over the course of 4 d. Finally, flow cytometry was used to show that the fluorescence from MitoSOX™ Red, a selective indicator of superoxide in mitochondria, was statistically similar in both control cells and cells incubated in DM-SWNTs. The combined results indicate that under our sample preparation protocols and assay conditions, CoMoCAT DM-SWNT dispersions are not inherently cytotoxic to HeLa cells. We conclude with recommendations for improving the accuracy and comparability of carbon nanotube (CNT) cytotoxicity reports.
doi:10.1186/1477-3155-5-8
PMCID: PMC2131758  PMID: 17956629
24.  Effect of Purity and Substrate on Field Emission Properties of Multi-walled Carbon Nanotubes 
Nanoscale Research Letters  2007;2(7):331-336.
Multi-walled carbon nanotubes (MWNT) have been synthesized by chemical vapour decomposition (CVD) of acetylene over Rare Earth (RE) based AB2(DyNi2) alloy hydride catalyst. The as-grown carbon nanotubes were purified by acid and heat treatments and characterized using powder X-ray diffraction, Scanning Electron Microscopy, Transmission Electron Microscopy, Thermo Gravimetric Analysis and Raman Spectroscopy. Fully carbon based field emitters have been fabricated by spin coating a solutions of both as-grown and purified MWNT and dichloro ethane (DCE) over carbon paper with and without graphitized layer. The use of graphitized carbon paper as substrate opens several new possibilities for carbon nanotube (CNT) field emitters, as the presence of the graphitic layer provides strong adhesion between the nanotubes and carbon paper and reduces contact resistance. The field emission characteristics have been studied using an indigenously fabricated set up and the results are discussed. CNT field emitter prepared by spin coating of the purified MWNT–DCE solution over graphitized carbon paper shows excellent emission properties with a fairly stable emission current over a period of 4 h. Analysis of the field emission characteristics based on the Fowler–Nordheim (FN) theory reveals current saturation effects at high applied fields for all the samples.
doi:10.1007/s11671-007-9067-3
PMCID: PMC3246377  PMID: 21798103
Multi-walled carbon nanotubes; DyNi2alloy hydride; Spin coating; Dichloro ethane; Graphitized carbon paper; CNT field emitter; Fowler–Nordheim theory
25.  Preparation of Solid Phase Microextraction (SPME) Probes through Polyaniline Multiwalled Carbon Nanotubes (PANI/MWCNTs) Coating for the Extraction of Palmitic Acid and Oleic Acid in Organic Solvents 
A fiber coating from polyaniline (PANI) was electrochemically prepared and employed for Solid phase micreoextraction (SPME). The PANI film was directly electrodeposited on the platinum wire surface using cyclic voltametry (CV) technique. The same method was applied for the preparation of SPME fiber coated by polyaniline multiwalled carbon nanotubes (PANI/MWCNTs) composite. The concentration of sulfuric acid for electropolymerization was 0.1 M in the presence of 0.045 M aniline in aqueous solution. For the electrodeposition of PANI/MWCNT composite, 4 μg/mL of MWCNTs was dispersed into the solution. Film coating was carried out on the platinum wire by repetitive cycling of potentials between 0 and 1.0 V at the scan rate of 0.05 V/s. The applicability of these coatings were assessed through employing a laboratory-made SPME injecting device and gas chromatography with mass spectrometry (GC-MS) for the extraction of palmitic acid and oleic acid from chloroform.
The developed method proved to be simple and easy, offering high reproducibility. Both PANI coated and PANI/CNT coated probes had the ability to concentrate palmitic acid and oleic acid on their coating and produced strong signals in GC-MS chromatograms. In the meantime, PANI/CNT coated SPME probes produced signals which were stronger than those produced by PANI coated SPME probes. The amount of extracted palmitic acid and oleic acid from chloroform by the PANI/MWCNTs coating was about 6 and 12 times higher than the amount extracted by plane PANI SPME fibers respectively.
It could be suggested that the composite material with CNTs has both an increased surface area and an elevated absorptive capacity which leads to this overall increase in extracted palmitic acid and oleic acid.
PMCID: PMC3813084  PMID: 24250460
Solid-phase microextraction; Multiwalled carbon nanotubes; Cyclic voltammetry; Gas chromatography-mass spectrometry

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