Self filling of Ni nanoparticles in amorphous AlN nanotubes and its field emission property

Unique aluminum nitride amorphous nanotubes filled with Ni nanoparticles have been successfully synthesized through the reaction of NH₃ over Ni-Al thin film at 1000 °C, which is similar to the extended vapor-liquid-solid technique. The X-ray diffraction and high-resolution transmission electron microscopic results are in good agreement with the amorphous nature of AlN nanotubes and crystallinity of Ni nanoparticles. The AlN nanotubes were having average diameter 35 nm and length ∼4 μm, whereas the Ni nanoparticles were having 5 nm in diameter. The unique structure showed excellent field emission property and high electrical conductivity ∼0.43 kmho/m at room temperature. The mechanism of good field emission property has been explained in detail.     

Synthesis of Y-junction carbon nanotubes within porous anodic aluminum oxide template

Y-junction carbon nanotubes with the average diameter about 200 nm were successfully synthesized within porous anodic aluminum oxide template, which was prepared by anodic anodizing aluminum sheet in 1.0 mol/l H₃PO₄ solution at a constant anodization voltage 90 V.     

Study on effects of substrate temperature on growth and structure of alignment carbon nanotubes in plasma-enhanced hot filament chemical vapor deposition system

Alignment carbon nanotubes (ACNTs) were synthesized on silicon substrate coated with Ni catalyst film and Ta buffer layer by plasma-enhanced hot filament chemical vapor deposition using CH₄, NH₃, and H₂ as the reaction gas, and they were investigated by scanning electron microscopy and transmission electron microscopy. It is found that the diameter of the bamboo-structured ACNTs is increased from 62 to 177 nm when the substrate temperature was changed from 626 to 756 °C. Their growth rate is enhanced by the substrate temperature in a range of 626-683 °C and it is reversely reduced with the substrate temperature after the substrate temperature is over 683 °C. Beginning with wetting phenomenon, the effects of the substrate temperature on the structure and growth rate of the ACNTs are analyzed.     

From crystalline V2O5 to nanostructured vanadium oxides using aromatic amines as templates

Nanoneedles, nanorods of B-VO₂, and vanadium oxide nanotubes with high crystallinity were synthesized via a one-step hydrothermal treatment using crystalline V₂O₅ as a precursor and aromatic amines (C₆H₅-(CH₂)_n-NH₂ with n=0, 1, 3) as structure-directing templates. Samples were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray powder diffraction (XRD), thermal analysis, nitrogen adsorption/desorption isotherms and infrared spectroscopy. Nanoneedles, 0.5-5 μm in length and about 50 nm in average diameter and VO₂(B) nanorods about 20-100 nm wide and up to 2.5 μm long, have been obtained. The inner and the outer diameters of the vanadium oxide nanotubes vary, respectively, between 15-25 and 70-100 nm with a length up to 4 μm.     

Effect of Ni, Pd and Ni-Pd nano-islands on morphology and structure of multi-wall carbon nanotubes

In this research, the effect of Ni, Pd and Ni-Pd catalysts have studied on morphology and structure of synthesized multi-wall carbon nanotubes (MWCNTs). Initially, thin films of Ni (with two thicknesses of 10 and 20 nm), Pd/Ni (5/10 nm) and Pd (10 nm) were deposited as catalysts on SiO₂ (60 nm)/Si(1 0 0) substrates, using dc magnetron sputtering technique. The deposited films were annealed at 900 °C in ammonia environment for 45 min, in order to obtain nano-structured catalyst on the surface. Using scanning electron microscopy (SEM), the average size of Ni nano-islands (synthesized by the 10 and 20 nm Ni films), Pd and Ni-Pd nano-islands were measured about 55, 110, 45 and 50 nm, respectively. According to X-ray photoelectron spectroscopy analysis (XPS), the ratio of Ni/Pd on the surface was about 3 for the bilayer sample. The CNTs were synthesized on the nano-island catalysts at 940 °C in CH₄ ambient using a thermal chemical vapor deposition method. The results revealed that average diameter of the CNTs were about 70, 110, 120 nm for Ni, Ni-Pd and Pd catalysts, respectively. Raman spectra of the MWCNTs showed that intensity ratio of two main peaks located in the range of 1550-1600 and 1250-1450 cm⁻¹ (as a quality factor for the CNTs) for Ni, Pd and Ni-Pd catalysts were 1.42, 0.91 and 0.85, respectively. Therefore, based on our data analysis, although addition of Pd to Ni catalyst caused a considerable reduction in the quality of the grown MWCNTs as compared to the pure Ni catalyst, but it resulted in an enhancement in the methane decomposition rate. For the pure Pd catalyst samples, both a slow methane decomposition rate as compared with Ni-Pd catalyst samples and a poor quality of CNTs were observed as compared with the Ni catalyst, under similar experimental conditions.     

Synthesis and H2 sensing properties of aligned ZnO nanotubes

Aligned ZnO nanotubes with the outer radius of about 200 nm were synthesized by a two-step approach, which involves electrospinning and sputtering techniques. The ZnO nanotubes are polycrystalline hexagonal structure, indicted by XRD and TEM analysis. The ZnO nanotubes show sensing property to H₂. The sensor response of the aligned nanotubes to 100 ppm H₂ increases from 2.3 to 3.6 with the temperature increasing from 200 to 400 °C. Beside, the sensor response of the ZnO nanotubes increases compared with that of the ZnO film prepared under the same condition.     

Flame synthesis of carbon nanotubes for panel field emission lamp

Multi-walled carbon nanotubes (CNTs) were synthesized on the surfaces of Ni-alloy plated Fe-wires with the diameter of 2 mm using a conventional laboratory ethanol (C₂H₅OH) flame method at 560 °C. SEM showed that the product had bush-shaped micron-structures with diameters from 100 to 450 nm and lengths of over 1.0 μm. TEM revealed that the micron-structures were composed of multi-walled nanotube bundles with the diameters of about 50 nm. The test on the diode configuration field emission of the Fe-wire arrays was performed. The onset electric field was 2.95 V/μm and the emission current can reach 50 mA/cm² at an electric field of 9 V/μm. The average fluctuation of the emission current density was less than 7%. The result suggests that the field emission was uniform and the present technique was feasible to fabricate Panel Field Emission Lamp (PFEL) with arrays of carbon nanotubes. PFEL has the advantages of high luminescence as well as stability, and thus, it can be used to replace ordinary lights.     

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

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

Catalytic activity of Fe, Co and Fe-Co-MCM-41 for the growth of carbon nanotubes by chemical vapour deposition method

Iron, cobalt and a mixture of iron and cobalt incorporated mesoporous MCM-41 molecular sieves were synthesised by hydrothermal method and used to investigate the rules governing their nanotube producing activity. The catalysts were characterised by XRD and N₂ sorption studies. The effect of the catalysts has been investigated for the production of carbon nanotubes at an optimised temperature 750 °C with flow rate of N₂ and C₂H₂ is 140 and 60 ml/min, respectively for a reaction time 10 min. Fe-Co-MCM-41 catalyst was selective for carbon nanotubes with low amount of amorphous carbon with increase in single-walled carbon nanotubes (SWNTs) yield at 750 °C. Formation of nanotubes was studied using scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Raman spectroscopy. Transmission electron microscope and Raman spectrum was used to follow the quality and nature of carbon nanotubes formed and the graphitic layers and disordered band, which shows the clear evidence for the formation of SWNTs, respectively. The result propose that the diameter of the nanotubes in the range of 0.78-1.35 nm. Using our optimised conditions for this system, Fe-Co-MCM-41 showed the best results for selective SWNTs with high yield when compared with Fe-MCM-41 and Co-MCM-41.     

An optical fiber glass containing PbSe quantum dots

An optical fiber material, sodium-aluminum-borosilicate glass doped with PbSe quantum dots (QDs) is synthesized by a high-temperature melting method. Crystallization, size distribution and absorption-photoluminescence (PL) of this material are observed by XRD, TEM, and spectrometer respectively. The obtained results indicate that the glass contains QDs in diameter of 6-13 nm depending on the heat-treatment temperature and with a higher doped concentration than those available. It shows an enhanced PL, widened FWHM (275-808 nm), obvious Stokes shift (20-110 nm), with the PL peak wavelength located within 1676-2757 nm depending on the size of QD. The glass is fabricated into an optical fiber in diameter of 10-70 μm and length of 1 m, with pliability and ductility similar to usual SiO₂ fibers. It can be easily fused and spliced with SiO₂ fibers due to a small difference of melting point between them. Characterized by high doped concentration and broad FWHM, this study suggests that the glass can be applied to designing novel broadband fiber amplifiers working in C-L waveband.     

Field emission properties of carbon nanotubes grown on silicon nanowire arrays

Carbon nanotubes are synthesized on the silicon nanowire arrays which are fabricated on silicon substrate by chemical vapor depositing SiCl₄ and H₂ gases in the presence of Au catalysts. The silicon nanowires are single-crystal with lengths up to 100 μm and diameters ranging from 50 to 500 nm. The tangled carbon nanotubes are grown directly from the surface of Si nanowires. The field emission properties of the carbon nanotubes are investigated at the gap of 200 μm. The low turn on and threshold fields are obtained. The stabilization of the emission currents is also presented.     

Preparation of visible-light responsive PF-codoped TiO2 nanotubes

Fabrication of PF-codoped TiO₂ nanotubes was carried out using a one-step electrochemical anodization process by tailoring the composition of the electrolyte with the aim of PF-codoping to extend the optical absorption of TiO₂ to the visible-light region. The as-prepared PF-codoped TiO₂ nanotubes were characterized by SEM, XPS, and UV-vis diffuse reflectance absorption spectra (DRS). The results showed that the tube diameter of the nanotubes was approximately 100 nm and the tube length was approximately 510 nm. The phosphorus and fluorine were successfully doped into TiO₂ nanotubes, as evidenced by XPS. Moreover, the PF-codoped samples displayed remarkably strong visible-light response.     

One-dimensional polyaniline nanostructures synthesized by interfacial polymerization in a solids-stabilized emulsion

One-dimensional polyaniline nanostructures were synthesized by interfacial polymerization in a solids-stabilized oil/water emulsion for the first time. The products were characterized with TEM, FTIR and UV-vis. FTIR analyses proved the polyaniline synthesized were of emeraldine salt form; the results of TEM showed that when MgCO₃ and CaCO₃ particles were used as emulsifiers, polyaniline nanofibers with an average diameter of 33 nm and nanotubes with an average outer diameter of 28 nm were obtained, respectively. Comparing to ordinary interfacial polymerization approach, our new route needed much less amount of oil phase and shorter polymerization time. A possible mechanism for the formation of one-dimensional polyaniline nanostructures was suggested.     

Synthesis and field-emission of aligned SnO2 nanotubes arrays

Aligned tin dioxide (SnO₂) nanotubes have been synthesized by high-frequency inductive heating. Nanotubes with high yield were grown on silicon substrates in less than 5 min, using SnO₂ and graphite as the source powder. Scanning electron microscopy and transmission electron microscopy showed nanotube with diameters from 50 to 100 nm and lengths up to tens of mircrometers. The SnO₂ nanotubes synthesized under the optimum condition have better field-emission characteristics. The turn-on field needed to produce a current density of 10 μA/cm² is found to be 1.64 V/μm. The samples show good field-emission properties with a fairly stable emission current. This type of SnO₂ nanotubes can be applied as field emitters in displays as well as vacuum electric devices.     

Standing or lying C70s encapsulated in carbon nanotubes with different diameters

Single-walled carbon nanotubes (SWNTs) encapsulating C₇₀s, so-called C₇₀ peapods, were synthesized in high yield by a vapor-phase doping method. Raman spectra, high resolution transmission electron microscopy (HRTEM), and selected area electron diffraction (SAED) measurement indicate that the tube diameter is one of the important factors to determine the orientation of C₇₀ molecules inside the SWNTs. SWNTs with different diameters give different alignment of C₇₀ molecules. The lying orientation is favorable over the standing orientation in thin nanotube, i.e. 1.36 nm nanotubes, whereas the standing orientation is favorable in thick nanotubes, i.e. 1.49 and 1.61 nm nanotubes.     

Fabrication of well-aligned CdS nanotubes by CVD-template method

Well-aligned CdS nanotubes have been synthesized within the nanochannels of the porous anodic alumina (PAA) membranes by pyrolyzing cadmium bis(diethyldithiocarbamate) [Cd(S₂CNEt₂)₂] at 400 °C. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) show that the CdS nanotubes are highly ordered with uniform diameter in range of 80-150 nm and the length up to tens of microns. X-ray diffraction (XRD), Raman spectrum, energy-dispersive spectroscopy (EDS) and selected-area electron diffraction (SAED) demonstrate that the nanotubes are composed of pure hexagonal phase polycrystalline CdS. The synthetic route can, in principle, be extended to fabricate other nanotubes of a wide range of semiconductors.     

Development and characterization of a novel silicon-based glassy composite as an anode material for Li-ion batteries

A novel silicon-based glassy composite anode material with high initial coulombic efficiency and long cycling performance for lithium-ion batteries was synthesized by a wet mechanochemical reduction method. The in situ formed Si particles with size of 5-10 nm were uniformly distributed in the glassy matrices formed by B₂O₃ and P₂O₅. The as-prepared composite electrode revealed an initial charge and discharge capacity of 432.7 and 514.4 mAh g^− 1, respectively, with an initial coulombic efficiency of 84%. After 100 cycles, the reversible capacity retention rate was still up to 97%, meaning a favorable cycling stability.     

Synthesis,photophysical properties,and photocatalytic applications of Bi doped NaTaO3 and Bi doped Na2Ta2O6 nanoparticles

Phase formation and photophysical properties of bismuth doped sodium tantalum oxide (perovskite, defect pyrochlore) nanoparticles prepared by a hydrothermal method were studied in detail. It was revealed that the synthesis conditions like NaOH concentration and bismuth precursor (NaBiO₃·2H₂O) markedly affect the crystal structure of sodium tantalum oxide. At low NaOH concentration and high bismuth precursor (NaBiO₃·2H₂O) content, Bi doped Na₂Ta₂O₆ (defect pyrochlore) phase was predominantly formed, while at higher NaOH concentration, Bi doped NaTaO₃ (perovskite) phase was formed. It was observed that the defect pyrochlore (Bi doped Na₂Ta₂O₆) phase was formed and stabilized by the presence of dopant precursor (NaBiO₃·2H₂O). The chemical analysis of the samples confirmed the doping of Bi³⁺ cations in both phases. Doping of bismuth enabled visible light absorption up to 500 nm in perovskite and defect pyrochlore type sodium tantalum oxide. Bi doped NaTaO₃ samples showed better performance for the photocatalytic degradation of rhodamine B than that of Bi doped Na₂Ta₂O₆, under visible light irritation (λ>420 nm). The present results shed light on phase formation of sodium tantalate and these results are useful in understanding properties of NaTaO₃ based compounds, synthesized by the hydrothermal method.     

Synthesis and photoluminescence properties of Sm-doped CaWO4 nanoparticles

The Sm³⁺-doped CaWO₄ nanoparticles were synthesized by hydrothermal method. The room temperature photoluminescence (PL) spectra of Sm³⁺-doped CaWO₄ nanoparticles doped with different Sm³⁺ concentrations under 405 nm excitation have been investigated. The PL spectra showed four strong emission peaks at 460, 571, 609, and 653 nm. The first emission peak at 460 nm could be due to a structural defect of the lattice, an oxygen-deficient WO₃ complex. The other three emissions at 571, 609, and 653 nm were due to the f-f forbidden transitions of the 4f electrons of Sm³⁺, corresponding to ⁴G_5/2→⁶H_5/2 (571 nm), ⁶H_7/2 (609 nm), and ⁶H_9/2 (653 nm), respectively. In addition, the optimum Sm³⁺ concentration in CaWO₄ nanoparticles for optical emission was determined to be 1.0%. The Sm³⁺⁴G_5/2→⁶H_7/2 (609 nm) emission intensity of Sm³⁺-doped CaWO₄ nanoparticles significantly increased with the increase of Sm³⁺ concentration, and showed a maximum when Sm³⁺ doping content was 1.0%. If Sm³⁺ concentration continued to increase, namely more than 1.0%, the Sm³⁺⁴G_5/2→⁶H_7/2 emission intensity would decrease. The present materials might be a promising phosphor for white-light LED applications.     

Tailoring the exchange bias of Ni/NiO nanogranular samples by the structure control

The exchange bias (EB) effect has been studied in Ni/NiO nanogranular samples obtained by annealing in H₂, at selected temperatures (200≤T_ann≤300 °C), NiO powder previously milled for 5, 10, 20 and 30 h. Both the as-milled NiO powders and the Ni/NiO samples have been analyzed by X-ray diffraction and the exchange bias properties have been investigated in the 5-200 K temperature range. The structure and the composition of the Ni/NiO samples can be satisfactorily controlled during the synthesis procedure by varying both T_ann and the milling time of the precursor NiO powders. In particular, by increasing this last parameter, the mean grain size of the NiO phase reduces down to the final value of 16 nm and the microstrain increases, which is consistent with an enhancement of the structural disorder. The structure of the milled NiO matrix strongly affects the process of nucleation and growth of the Ni nanocrystallites induced by the H₂ treatments, so that, T_ann being equal, the amount and the mean grain size D_Ni of the Ni phase vary substantially in samples having different milling times. Such features of the Ni phase determine the extent of the Ni/NiO interface and consequently the magnitude of the exchange field H_ex: the highest value (∼940 Oe) has been measured at T=5 K in a sample containing ∼7 wt% Ni and with D_Ni=19 nm. However, in Ni/NiO samples with very different structural characteristics and different values of H_ex at T=5 K, the EB effect vanishes at the same temperature (∼200 K) and the same thermal dependence of H_ex is observed. We consider that the evolution of the EB effect with temperature is ultimately determined by the microstructure of the Ni/NiO interface, which cannot be substantially modified by changing the synthesis parameters, milling time and T_ann.