Large-scale synthesis of tungsten oxide nanowires with high aspect ratio

Through the controlled removal of surfactant from the presynthesized mesolamellar precursor (WO-L) at elevated temperature, tungsten oxide nanowires with diameters ranging from 10 to 50 nm and lengths up to several micrometers were obtained on a large scale. The structure, morphology, and composition of the nanowires were characterized by the XRD, TEM, HRTEM, EDX, and Raman spectra.     

Fabrication of gold microtubes and microwires in high aspect ratio capillary arrays

In this communication, we describe the sequential deposition of materials in capillaries as a means to produce self-assembled three-dimensional gold microtubes, hollow gold microwires, and microtube and microwire arrays with unprecedented aspect ratios. The initial application of this technique is the fabrication of an array of microwires within a silica capillary array. The physical characteristics of these microwires are characterized via SEM, electrochemistry, and electrogenerated chemiluminescence emission.     

A novel catalyst-free synthesis of vertically aligned silicon nanowire-carbon nanotube heterojunction arrays for high performance electron field emitters

A novel, catalyst-free strategy for the direct synthesis of vertically aligned silicon nanowire-carbon nanotube (SiNW-CNT) heterojunction arrays is presented. Such a heterojunction with the junction area in the nanoscale displays enhanced field emission characteristics at low turn-on field, with a nearly three times increase in the field enhancement factor.     

Design of experiment for optimization of plasma-polymerized octafluorocyclobutane coating on very high aspect ratio silicon molds

As-fabricated deep reactive ion etched (DRIE) silicon mold with very high aspect ratio (>10) feature patterns is unsuitable for poly(dimethylsiloxane) (PDMS) replication because of the strong interaction between the Si surface and the replica and the corrugated mold sidewalls. The silicon mold can be conveniently passivated via plasma polymerization of octafluorocyclobutane (C4F8), which is also employed in the DRIE process itself, to enable the mold to be used repeatedly. To optimize the passivation conditions, we have undertaken a Box-Behnken experimental design on the basis of three passivation process parameters (plasma power, C4F8 flow rate, and deposition time). The measured responses were fluorinated film thickness, demolding status/success, demolding force, and fluorine/carbon ratio on the fifth replica surface. The optimal passivation process conditions were predicted to be an input power of 195 W, a C4F8 flow rate of 57 sccm, and a deposition time of 364 s; these were verified experimentally to have high accuracy. Demolding success requires medium-deposited film thickness (66-91 nm), and the thickness of the deposited films correlated strongly with deposition time. At moderate to high ranges, increased plasma power or gas flow rate promoted polymerization over reactive etching of the film. It was also found that small quantities of the fluorinated surface were transferred from the Si mold to the PDMS at each replication, entailing progressive wear of the fluorinated layer.     

Enhanced electron field emission from ZnO nanoparticles-embedded DLC films prepared by electrochemical deposition

ZnO nanoparticles-embedded diamond-like amorphous (DLC) carbon films have been prepared by electrochemical deposition. Transmission electron microscopy (TEM) and high-resolution TEM (HRTEM) results confirm that the embedded ZnO nanoparticles are in the wurtzite structure with diameters of around 4 nm. Based on Raman measurements and atomic force microscope (AFM) results, it has been found that ZnO nanoparticles embedding could enhance both graphitization and surface roughness of DLC matrix. Also, the field electron emission (FEE) properties of the ZnO nanoparticles-embedded DLC film were improved by both lowering the turn-on field and increasing the current density. The enhancement of the FEE properties of the ZnO-embedded DLC film has been analyzed in the context of microstructure and chemical composition.     

Two-step synthesis of high aspect ratio gold nanorods

We describe a very simple, two-step synthetic method to prepare gold nanorods with extremely high aspect ratios (> 20) and average lengths of more than 1000 nm. The method is based on a seed-mediated growth in presence of the surfactant cetyltrimethylammonium bromide. The length and aspect ratios of the nanorods can be manipulated by varying the surfactant concentration.     

Microwave-assisted synthesis of high aspect ratio ruthenium nanorods

<正>Poly(N-vinyl-2-pyrrolidone)(PVP)-stabilized ruthenium nanorods with high aspect ratio by refluxing ruthenium(Ⅲ) chloride in n-propanol have been successfully prepared by means of a facile and rapid microwave heating for the first time.The structure and morphology of the obtained products were characterized by transmission electron microscopy(TEM),select area electron diffraction(SAED),ultraviolet-visible spectrophotometry(UV-vis),X-ray photoelectron spectroscopy(XPS) and Fourier transform spectroscopy(FT-IR).XPS analysis reveals that the nanorods were in the metallic state.TEM images showed that ruthenium nanorods had an obvious one-dimensional structure with the aspect ratio ranged from 5 to 40 nm and length up to 600 nm.SAED patterns indicated that the nanorods were single-crystalline with a hexagonal structure.     

Liquid crystalline properties of unsegmented and segmented polyurethanes synthesised from high aspect ratio mesogenic diols

A series of novel tetrad high aspect ratio mesogenic diol monomers 4-{[4-(n-hydroxyalkoxy)-phenylimino]-methyl}-benzoic acid 4-{[4-(n-hydroxyalkoxy)-phenylimino]-methyl}-phenyl ester were prepared with varying alkoxy spacer length (n=2,4,6,8,10) by reacting 4-formylbenzoic acid 4-formylphenyl ester and 4-(n-hydroxyalkoxy) anilines. Two series of thermotropic main chain liquid crystalline unsegmented polyurethanes (PUs) were obtained by the polyaddition of the mesogenic diols with hexamethylene diisocyanate (HMDI) and methylene bis(cyclohexylisocyanate) (H₁₂MDI) in dimethylformamide respectively. The effect of the incorporation of a third component namely polyol on the liquid crystalline properties of the polyurethanes was also studied. Linear segmented PUs were synthesised by a two-step block copolymerisation method. The PUs synthesised were based on six spacer mesogenic diol chain extender, soft segments poly(tetramethylene oxide)glycol (PTMG) (M_n= 650,1000,2000) and polycaprolactone diol (PCL) (M_n=530,1250,2000) of varying molecular weights and different diisocyanates including HMDI, H₁₂MDI and methylene bis(phenylene isocyanate) (MDI). Structural elucidation was carried out by elemental analysis, fourier transform infra red (FT-IR), nuclear magnetic resonance (¹H NMR and ¹³C NMR) spectroscopy. Inherent viscosity of the unsegmented polymers measured in methanesulphonic acid at 26°C was in the range of 0.13 - 0.65 dL/g while the molecular weights and molecular weight distribution of the segmented polyruethanes was determined using gel permeation chromatography (GPC). Mesomorphic properties were studied by differential scanning calorimetry (DSC) and hot stage polarising optical microscopy and the thermal stability was determined by thermogravimetric(TG)analysis. The monomeric diols and the polyurethanes exhibited nematic texture and good mesophase stability. It was observed that the partial replacement of the mesogenic diol by the polyol of varying molecular weights influenced the phase transitions and the occurrence of mesophase textures. The phase transition temperatures of the investigated polyurethanes showed dependence on the chain length of the soft segment and on the content of the mesogen moiety. A higher content of mesogenic moiety was needed to obtain liquid crystalline property when the soft segment length was increased as observed in the case of PTMG. Grained and threaded textures were observed depending on the molecular weight of the soft segment, the mesogen content and the diisocyanate. The stress-strain analyses showed that the polymers bused on high molecular weight PTMG soft segment have elastomeric property while the PCL based PUs displayed no elastomeric property.     

Effect of slot aspect ratio on droplet formation from silicon straight-through microchannels

We recently proposed a novel technique for preparing monodisperse emulsions using an array of microfabricated through-holes with an oblong section; we called this array a straight-through microchannel (MC). This paper reports how the slot aspect ratio of the straight-through MC affects droplet formation characteristics. Straight-through MCs with different slot aspect ratios and equivalent diameters of about 20 microm were used. Experimental observation showed that slot aspect ratios exceeding a threshold of approximately 3 were needed to successfully prepare monodisperse emulsions with coefficients of variation below 2%.     

Synthesis and dispersion of isolated high aspect ratio gold nanowires

We report the assembly properties of high density and high aspect ratio metal nanowire arrays (Au, Cu and Ag with diameters ranging from 40 to 250 nm) after release from the anodic alumina oxide (AAO) templates. Individual Ag and Cu nanowires were observed following release from the template, however, in the case of gold nanowires, the dispersion was dependent on size and aspect ratio. 40-100 nm gold wires aggregated to form bundles or disordered mats. We show that a simple cyanide-mediated release from the AAO template, results in isolated dispersion of wires even for the smallest wire diameters. Possible stabilising mechanisms for observed tendency of nanowires dispersion are discussed.     

Fabrication and characterization of smooth high aspect ratio zirconia nanotubes

In the present work, we report formation of high aspect ratio zirconia nanotubes by electrochemical anodization of zirconium in a 1 M (NH₄)₂SO₄ electrolyte containing 0.5 wt% NH₄F. Highly self-organized zirconia nanotubes can be formed with a diameter of ≈50 nm and a length of ≈17 μm, i.e. with an aspect ratio of more than 300. The nanotubes show a distinct smooth and straight morphology. XRD investigation reveals that the nanotubes have a cubic crystalline structure directly after anodization, that is, without any further annealing.     

Solvothermal synthesis of uniform and high aspect ratio of CdS nanowires and their optical properties

Uniform and high aspect ratio CdS nanowires (NWs) were successfully synthesized by the solvothermal reaction of the solution containing Cd(NO₃)₂, (NH₄)₂S and ethylenediamine (NH₂(CH₂)₂NH₂). In this research, the effects of molar contents of the stating materials, reaction temperatures and lengths of time on phase, vibration modes, morphologies, and optical properties of the as-synthesized products were studied using XRD, Raman spectroscopy, SEM, TEM, SAED, HRTEM, UV–vis spectroscopy and PL spectroscopy. They were found to be controlled by the contents of the stating materials, reaction temperatures and lengths of time. Mixed nanoparticles and short nanorods of CdS were synthesized by the 200 °C and 24 h solvothermal reaction of the solutions containing 0.0001–0.0050 mol of the starting materials. Upon increasing the content of the starting materials to 0.0100 mol, the completely uniform CdS NWs with aspect ratio of >250 were synthesized.     

Effect of ac electrodeposition conditions on the growth of high aspect ratio copper nanowires in porous aluminum oxide templates

The effect of several deposition parameters on the uniformity of copper electrodeposition through the alumina barrier layer into porous aluminum oxide templates grown in sulfuric or oxalic acid was systematically investigated. A fractional factorial design of experiment was conducted to find suitable deposition conditions among the variables: frequency, voltage, pulsed or continuous deposition, electrolyte concentration, and barrier layer thinning voltage. Continuous ac sine wave deposition conditions yielded excellent uniformity of pore-filling but damaged the porous aluminum oxide templates when deposition was continued to grow bulk copper on the surface. Pulsed electrodeposition yielded comparable uniformity of pore-filling and no damage to the porous aluminum oxide templates, even when bulk copper was deposited on them. Further optimization of pulsed deposition conditions was accomplished by comparing square and sine waveforms and pulse polarity. Pulsed square waveforms produced better pore-filling than pulsed sine waveforms. For sine wave depositions, the oxidative/reductive pulse polarity was more efficient than the commonly used reductive/oxidative pulse polarity. For square wave depositions into sulfuric acid grown pores, the reductive/oxidative pulse polarity produces more uniform pore-filling, likely as a result of enhanced resonant tunneling through the barrier layer and reoxidation of copper in faster filling pores.     

In situ generation of high aspect ratio silica particles in polypropylene

Polypropylene/silica microcomposites with high aspect ratio silica fillers were in situ generated into a molten polypropylene (PP) matrix. The synthesis of the inorganic domains are based on hydrolysis-condensation reactions of both alkoxysilanes precursors, the tetraethoxysilane (TEOS) and the Dynasil^? 40 (composed of TEOS and partially condensed TEOS with residual ethoxy groups) respectively. The sol?Cgel reactions kinetics studied at room temperature into an acid hydroalcoholic medium for several conditions of pH associated to the processing conditions were the keys factors to control the deformability of the inorganic droplets. Thanks to a shearing hot stage coupled with an optical microscope, silica needles were obtained with a Dynasil^? 40 solution treated 120?min at pH?=?3 in presence of 4?g of ethanol and then placed between two slices of PP in the stage. The deformation of the droplets were then observed once the material was molten and a shearing applied. On the contrary, no deformation was possible with TEOS precursors solutions. The results transposed to the microextruder process equipped at the die with a drawing line allowed to obtain a well pronounced elongated shape of the silica particles dispersed in the polypropylene matrix.     

Simulation and investigation of factors affecting high aspect ratio UV embossing

UV embossing is a replication method whereby an UV-curable polymer is pressed against a patterned mold and cured with UV irradiation, resulting in a patterned polymeric substrate. High aspect ratio UV embossing will find diverse applications in tissue engineering, micro-optics, display technologies, and sensors. Demolding of an UV-embossed polymer pattern with aspect ratio of 5 from the mold has previously been demonstrated experimentally. In this paper, parameters that affect the demolding process have been identified and investigated. They include cross-linking shrinkage during curing by UV irradiation, modulus of cured polymer, interfacial fracture strength and toughness, and loading method during demolding. Shrinkage is an important parameter, and an optimum level of shrinkage to avoid breakage of the embossing during demolding was found to exist. This optimum level is that at which the maximum stress (sigma(1)max) experienced by the polymer during demolding is minimized. The micromechanics of demolding was found to be different for shrinkage values lower or larger than the optimum value.     

Hydrothermal synthesis of hexagonal WO3 nanowires with high aspect ratio and their electrochemical properties for lithium-ion batteries

One dimensional WO₃ nanowires with high aspect ratio of >200 were synthesized by hydrothermal method. The effects of reaction temperature and time on phase and morphologies were studied and discussed. In this research, a suitable hydrothermal condition is at 200°C for 48 h. XRD, SEM, and TEM results show that the product is hexagonal WO₃ phase with diameter of 25 nm and several ten micrometers long with growth in the c direction. The electrochemical properties were tested for rechargeable lithium batteries. The WO₃ NWs electrode exhibits a stability trend over the 30 cycle testing. Some long-term activation process is attributed to the WO₃ NWs electrode during charge/discharge reaction.

     

Synthesis of high aspect ratio quantum-size CdS nanorods and their surface-dependent photoluminescence

Colloidal CdS nanorods with diameters near 4 nm and narrow size distributions ( approximately +/-10%) were synthesized up to 300 nm long by a sequential reactant injection technique that utilizes phosophonic acids as capping ligands. The phosphonic acid strongly passivates the nonpolar CdS surfaces and sequential reactant injection provides controlled CdS formation kinetics to enable heterogeneous and facet-selective CdS deposition on the more reactive {002} surfaces. With this process, the nanorod length can be systematically increased by increasing reactant addition to extend nanorod growth. The phosphonic acid concentration, however, is quite important, as "low" concentrations allow radial deposition and branching to occur. These high aspect ratio (>100) CdS nanorods luminesce with relatively high efficiencies of 10.8% quantum yield at room temperature. The luminescence, however, mostly arises from trap-related recombination, and the emission is significantly red-shifted from the absorption edge. Various surface passivation treatments were explored to eliminate trap emission and increase the luminescence quantum yield. Thiol and amine passivation both significantly reduced trap emission and enhanced band-edge emission, but the total luminescence quantum yields dropped significantly, with a maximum measured value of 1.5% for the amine-passivated CdS nanorods.     

Solution-phase synthesis of single-crystalline magnetic nanowires with high aspect ratio and uniformity

Single-crystalline Fe3O4 nanowires with uniform diameters and the largest aspect ratio (>500) were prepared by a one-step sol-gel process in the presence of ethylene glycol and poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol).