Electrochemical synthesis of ordered CdTe nanowire arrays

Semiconductor CdTe nanowire arrays embedded in the nanochannels of the porous anodic alumina (PAA) template have been prepared by using a potentiostatic electrochemical deposition method. The morphology and structure of the CdTe nanowire arrays have been characterized by X-ray powder diffraction, transmission electron microscopy, and high-resolution transmission electron microscopy. It is found that the CdTe nanowires with diameters and lengths of about 60 nm are single-crystalline with cubic phase structure, uniformly and continuously embedded in the nanochannels of the PAA template. X-ray energy-dispersion analysis and X-ray photoelectron spectroscopy analysis indicate that stoichiometric CdTe was formed. The growth mechanism of the CdTe nanowires is also discussed. Received: 11 June 2002 / Accepted: 2 July 2002 / Published online: 8 January 2003 RID="*" ID="*"Corresponding author. Fax: +86-551/559-1434, E-mail: aiwuzhao@yahoo.com.cn     

The synthesis of highly oriented GaN nanowire arrays

Highly oriented GaN nanowire arrays have been achieved by the catalytic reaction of gallium with ammonium. The resulting materials were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM) and selected-area electron diffraction (SAED). SEM images show that the resulting materials are nanowire arrays with a uniform length of about 10 μm. XRD, EDS, TEM and SAED indicate that the nanowire arrays are single-crystal hexagonal GaN with a wurtzite structure. They have diameters of 10 to 20 nm. Received: 2 October 2002 / Accepted: 7 October 2002 / Published online: 17 December 2002 RID="*" ID="*"Corresponding author. E-mail: wwwangjc@sina.com     

Large-scale synthesis of SnO2 nanobelts

Tin dioxide (SnO₂) nanobelts have been successfully synthesized in bulk quantity by a simple and low-cost process based on the thermal evaporation of tin powders at 800 °C. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) observations reveal that the nanobelts are uniform, with lengths from several-hundred micrometers to a few millimeters, widths of 60 to 250 nm and thicknesses of 10 to 30 nm. X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDX) and selected-area electron diffraction analysis (SAED) indicate that the nanobelts are tetragonal rutile structure of SnO₂. The SnO₂ nanobelts grow via a vapor–solid (VS) process. Received: 3 June 2002 / Accepted: 10 June 2002 / Published online: 10 September 2002 RID="*" ID="*"Corresponding author. Fax: +86-551/559-1434, E-mail: gwmeng@mail.issp.ac.cn     

Growth and morphologies of large-scale SnO2 nanowires, nanobelts and nanodendrites

Single-crystalline SnO₂ nanowires, nanobelts and nanodendrites were synthesized by a simple gas-reaction route on a large scale at 900 °C. They were characterized by means of X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM) and selected-area electron diffraction (SAED). FE-SEM images showed that the products consisted of nanowires, nanobelts and nanodendrites that represent a novel morphology reported for the first time. XRD, SAED and EDS indicated that they were single-crystalline tetragonal SnO₂. The influence of experimental conditions on the morphologies of the products is discussed. Received: 3 June 2002 / Accepted: 10 June 2002 / Published online: 10 September 2002 RID="*" ID="*"Corresponding author. Fax: 86-10/82649531, E-mail: xlchen@aphy.iphy.ac.cn     

Copper nanowire arrays for infrared polarizer

A micropolarizer of copper nanowire arrays within anodic alumina membrane (AAM) was fabricated by anodization of pure Al foil and electrodeposition of Cu, respectively. X-ray diffraction, scanning electron microscopy and transmission electron microscopy investigations reveal that the ordered Cu nanowires are essentially single crystal, and have an average diameter of 90 nm. Spectrophotometer measurements show that the copper nanowire arrays embedded in AAM can only transmit polarized light vertical to the wires. An extinction ratio of 24 to 32 dB and an average insertion loss of 0.5 dB in the wavelength range of 1 to 2.2 μm were obtained, respectively. Therefore Cu nanowire/AAM can be used as a wire grid type micropolarizer. Received: 28 January 2002 / Accepted:17 May 2002 / Published online: 22 November 2002 RID="*" ID="*"Corresponding author. Fax: +86-551/559-1434, E-mail: ytpang@263.net     

Structural and optical properties of nanophase zinc oxide

Nanophase zinc oxide samples were synthesized by a two-step solid-state reaction method. The phase structure and microstructure were investigated by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The vibrational Raman spectra were compared with those from the bulk and their grain size dependence was also examined. Their photoelectric behavior was studied by X-ray photoelectron spectroscopy (XPS). The peaks at 1044.5 and 1021.4 eV were recorded as corresponding to the respective binding energies of Zn 2p_1/2 and Zn 2p_3/2, and the photoelectron spectrum of O 1s in the as-prepared powder was located at 531.2 eV. A strong visible emission centered at 580 nm was clearly observed in the nanosized zinc oxide at room temperature. Photoluminescence (PL) spectra were investigated as a function of grain size after different heat treatments. The origin of the luminescence is attributed to the recombination of electrons in singly occupied oxygen vacancies with photoexcited holes in the valence band. Received: 30 June 2001 / Accepted: 20 February 2002 / Published online: 3 June 2002 RID="*" ID="*"Corresponding author. Fax: +86-25/359-5535, E-mail: mszhang@nju.edu.cn     

Filling boron nitride nanotubes with metals

The authors’ endeavors over the last few years with respect to boron nitride (BN) nanotube metal filling are reviewed. Mo clusters of 1–2 nm in size and FeNi Invar alloy (Fe ∼60 at. %; Ni ∼40 at. %) or Co nanorods of 20–70 nm in diameter were embedded into BN nanotube channels via a newly developed two-stage process, in which multi-walled C nanotubes served as templates for the BN multi-walled nanotube synthesis. During cluster filling, low-surface-tension and melting-point Mo oxide first filled a C nanotube through the open tube ends, followed by fragmentation of this filling into discrete clusters via O₂ outflow and C→BN conversion within tubular shells at high temperature. During nanorod filling, C nanotubes containing FeNi or Co nanoparticles at the tube tips were first synthesized by plasma-assisted chemical vapor deposition on FeNi Invar alloy or Co substrates, respectively, and, then, the nanomaterial was heated to the melting points of the corresponding metals in a flow of B₂O₃ and N₂ gases. During this second stage, simultaneous filling of nanotubes with a FeNi or Co melt through capillarity and chemical modification of C tubular shells to form BN nanotubes occurred. The synthesized nanocomposites were analyzed by scanning and high-resolution transmission electron microscopy, electron diffraction, electron-energy-loss spectroscopy and energy-dispersive X-ray spectroscopy. The nanostructures are presumed to function as ‘nanocables’ having conducting metallic cores (FeNi, Co, Mo) and insulating nanotubular shields (BN) with the additional benefit of excellent environmental stability. Received: 10 October 2002 / Accepted: 25 October 2002 / Published online: 10 March 2003 RID="*" ID="*"Corresponding author. Fax: +81-298/51-6280, E-mail: golberg.dmitri@nims.go.jp     

Low-threshold field electron emission of Si micro-tip arrays produced by laser ablation

Low-threshold field electron emission (FEE) is reported for periodic arrays of micro-tips produced by laser ablation of Si wafers. The best samples show emission at threshold fields as low as 4–5 V/μm for n-type Si substrates and of 1–2 V/μm for p-doped Si substrates, as measured with a flat-screen technique. Auger electron spectroscopy and X-ray electron spectroscopy reveal island-like deviation of the SiO₂ stoichiometry on the tip surfaces, with lateral dimensions of less than 100 nm. Microscopic studies using a special field-emission STM show that the emission originates from well-conducting regions of sub-micron size. The experimental data suggest FEE from the tip arrays by a geometric field enhancement of both the individual micro-tip and the narrow conducting channels in the tip body. Received: 3 May 2002 / Accepted: 1 July 2002 / Published online: 28 October 2002 RID="*" ID="*"Corresponding author. Fax: +7-095/135-82-34, E-mail: shafeev@kapella.gpi.ru     

Preparation of Mn<Subscript>3</Subscript>O<Subscript>4</Subscript> nanowires by calcining the precursor powders synthesized in a novel inverse microemulsion

Manganese oxide (hausmannite) nanowires were prepared by annealing precursor powders at a temperature of 800 °C for 3 h, which were produced in a novel inverse microemulsion (IμE) system. The microstructures of the as-prepared Mn₃O₄ nanowires were investigated by means of X-ray diffraction, transmission electron microscopy, and Raman spectra. It has been found that the Mn₃O₄ nanowires were relatively straight and their surfaces were smooth with a typical diameter of 75–150 nm. The formation mechanism of the Mn₃O₄ nanowires is discussed. Received: 30 May 2002 / Accepted: 7 October 2002 / Published online: 17 December 2002 RID="*" ID="*"Corresponding author. Fax: +86-25/359-5535, E-mail: wangqun@nju.edu.cn     

Influence of SnO2 coating and thermal annealing on the structure and luminescence properties of CuO nanorods

CuO-core/ SnO₂-shell one-dimensional nanostructures have been fabricated by thermal oxidation of a copper foil and then atomic layer deposition of SnO₂. The structure and optical properties of the nanostructures have been investigated by using scanning electron microscopy, transmission electron microscopy, X-ray diffraction, photoluminescence (PL) spectroscopy, and energy-dispersive X-ray analysis techniques. The nanostructures are found to have the form of nanorods, with the diameter of the CuO cores being in the range from a few tens to a few hundreds of nanometers, the thickness of the SnO₂ shells being ～15 nm, and with a length of a few tens of micrometers. The CuO cores and the SnO₂ shells of the as-synthesized nanorods have crystalline monoclinic CuO and amorphous SnO₂ structures, respectively, but the SnO₂ shells are found to crystallize to tetragonal SnO₂ on thermal annealing. The PL emission intensity of the CuO nanorods has been slightly increased by SnO₂ coating. The PL emission of the SnO₂-coated CuO nanorods is somewhat increased and the emission peak position is red-shifted from 550 to 580 nm by annealing in a reducing atmosphere. On the other hand, the PL emission is significantly increased and the emission peak position is shifted from 550 nm further to around 595 nm by annealing in an oxidative atmosphere. In addition, the origins of the PL enhancements in the nanorods by coating and annealing are discussed.     

Growth of a textured quasicrystalline phase in Ti-Ni-Zr films prepared by pulsed laser deposition

The preparation in thin film form of the known icosahedral phase in Ti-Ni-Zr bulk alloys has been investigated as a function of substrate temperature. Films were deposited by pulsed laser deposition on sapphire substrates at temperatures ranging from room temperature to 350 °C. Morphological and structural modifications have been followed by grazing-incidence and θ–2θ X-ray diffraction, transmission electron diffraction and imaging. Chemical composition has been analyzed by electron probe microanalysis. The in-depth variation of composition has been studied by secondary neutral mass spectroscopy. We show that pulsed laser deposition at 275 °C makes the formation of a 1-μm-thick film of Ti-Ni-Zr quasicrystalline textured nanocrystallites possible. Received: 7 June 2001 / Accepted: 18 February 2002 / Published online: 3 June 2002 RID="*" ID="*"Corresponding author. Fax: +33-3/8357-6300, E-mail: brien@mines.u-nancy.fr     

ZnO–CuO core–shell nanorods and CuO-nanoparticle–ZnO-nanorod integrated structures

ZnO–CuO core–shell nanorods and CuO-nanoparticle–ZnO-nanorod integrated structures were synthesized for the first time by a two-stage solution process. Scanning electron microscopy and high-resolution transmission electron microscopy show that the diameter and the length of the nanorods are around 60 and 800 nm, respectively. The morphologies of outer CuO could be varied from nanoparticles to nanoshells by adjusting the solvent and dipping processes of copper (II) nitrate solution. The CuO nanoparticles are single-crystalline or highly textured structures with size of around 30 nm. The CuO shell with thickness of around 10 nm is constructed of nanocrystals with sizes in the range of 3–10 nm embedded in an amorphous matrix. Room-temperature cathodoluminescence measurements of the CuO–ZnO nanocomposites exhibit relatively sharp ultraviolet emissions at 380 nm as well as broad green and yellow emissions at 500 and 585 nm. The p-CuO/n-ZnO one-dimensional nanocomposites are promising for optoelectronic nanodevice applications.     

In situ synthesis of mesoporous CdS nanoparticles in ternary cubic phase lyotropic liquid crystal

An in situ technique for the synthesis of CdS nanoparticles in a ternary lyotropic cubic phase liquid crystal has been carried out. The extremely viscous cubic phase liquid-crystal system consists of poly(oxyethylene)₁₀ nonyl phenol ether as non-ionic surfactant, octane as oil phase and an aqueous phase containing reactant ions (Cd²⁺ and S^2-). Thioacetamide (TAA) has been utilized as a source for slow release of sulfur in the in situ synthesis of CdS. Rheological results show that CdS nanoparticle growth did not disrupt the structure of the cubic phase liquid-crystal system. This indicates that homogenous synthesis of CdS in the liquid crystal had been achieved. The final products were characterized using X-ray photoelectron spectroscopy, thermal gravimetric analysis, transmission electron microscopy and UV-visible spectroscopy. It was found that the CdS nanoparticles formed have a mesoporous structure with a size dependent on the TAA decomposition aging time. Received: 29 March 2002 / Accepted: 4 September 2002 / Published online: 17 December 2002 RID="*" ID="*"Corresponding author. Fax: +603-8921/3257, E-mail: shahidan@pkrisc.cc.ukm.my     

Sub-ps laser microstructuring of soft X-ray Mo/Si multilayer gratings

The sub-picosecond laser microstructuring of multilayer gratings is presented in this paper. A micromachining system operating with a 0.5 ps KrF laser at 248 nm was used to etch grating structures with a groove width of 1–2 μm in Mo/Si and Si/Mo multilayers. Atomic force microscopy, scanning electron microscopy and X-ray reflectivity were used to characterize the microetched patterns. The ω-scans around the 1st Bragg maximum show symmetric satellites up to 3rd order, with positions corresponding to the grating period. The use of sub-picosecond laser pulses minimizes the thermally affected zone and enhances the quality of the etched features. Short pulse laser processing is advantageous for the fabrication of high spatial resolution microstructures required in X-ray optics. Received: 21 May 2002 / Accepted: 19 August 2002 / Published online: 15 January 2003 RID="*" ID="*"Corresponding author. Email: dpapa@iesl.forth.gr     

Orientation studies of Si-phthalocyanine sulfonic acids cast on SiOx substrates

Layers of dihydroxy silicon phthalocyanine tetrasulfonic acid and oligo-μ-oxo silicon phthalocyanine tetrasulfonic acid were prepared by solution-casting methods. The purity of the material was checked by X-ray photoemission spectroscopy. The orientation of the molecules in respect to the substrate plane was investigated by angle-dependent near-edge X-ray absorption fine-structure spectroscopy. The morphology was characterized by atomic force microscopy. Most samples exhibited a significant orientation that was accompanied by crystalline structures; others had no orientation at all with a dominant amorphous morphology. This behavior indicates that several preparation parameters affect the crystallinity and the orientation of the phthalocyanines. Received: 16 January 2002 / Accepted: 11 February 2002 / Published online: 3 May 2002 RID="*" ID="*"Corresponding author. Fax: +1-919/515-7331, E-mail: harald_ade@ncsu.edu RID="**" ID="**"Present address: Southern Illinois University, Physics, Mailcode 4401, Carbondale, IL 62901, USA     

Third-order nonlinear optical response of Au-core CdS-shell composite nanoparticles embedded in BaTiO<Subscript>3</Subscript> thin films

Au-core CdS-shell composite nanoparticles were synthesized by a direct self-assembly process and integrated into BaTiO₃ thin films. Characterization by transmission electron microscopy showed that the average diameter of these composite nanoparticles was about 8 nm. Using the femtosecond time-resolved optical Kerr effect method, we investigated the third-order nonlinear optical response of the Au@CdS nanoparticles embedded in the BaTiO₃ thin films at a wavelength of 800 nm. An ultrafast nonlinear response and a large effective third-order nonlinear susceptibility of χ⁽³⁾=7.7×10^-11 esu were observed. We attributed the enhancement of the third-order optical nonlinearity to a localized electric field effect originating from the core-shell structure under off-surface-plasmon resonance conditions. Received: 13 May 2002 / Revised version: 23 October 2002 / Published online: 3 April 2003 RID="*" ID="*"Corresponding author. Fax: +86-21/6510-4949, E-mail: sxqian@fudan.ac.cn     

Microstructural properties of bulk nanocrystalline Ag–Ni alloy prepared by hot pressing of mechanically pre-alloyed powders

A bulk nanocrystallined Ag50Ni alloy has been prepared by hot-pressing the mechanically pre-alloyed powders at 620 °C under a normal pressure of 58 MPa in vacuum. The microstructural characteristics of the alloy were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results of the precise determination of the lattice parameters of the phases in the powders and in the alloy by XRD show that, after mechanical alloying for 200 h, the solid solubility of Ag in Ni reaches 4.85±0.21 at %, while that of Ni in Ag reaches 0.84±0.30 at %. After hot pressing, the Ag- and Ni-rich phases in the alloy still show a certain degree of supersaturation, with a solid solubility of 0.45±0.11 at % of Ag in Ni. After further annealing of the alloy at 700 °C for 24 h, the solubility decreases to a value of 0.21±0.11 at % for Ag in Ni and to less than 0.1 at % for Ni in Ag. The grain size of the mechanically alloyed powders was of ca 6 nm. After hot pressing, the grain size of the alloy increased to 40–60 nm and then grew further to 100–110 nm after annealing. The influence of the variation of the grain size and the internal stress on the line breadth of the X-ray diffraction peaks has been evaluated in detail. Finally, the role of the nanocrystalline structure in the fast densification process of the powders is also discussed. Received: 12 September 2001 / Accepted: 18 Febraury 2002 / Published online: 10 September 2002 RID="*" ID="*"Corresponding author. Fax: +86-24/2389-3624, E-mail: wwt@icpm.syb.ac.cn     

Large-scale synthesis of rutile SnO2 nanorods

A high yield of tin oxide (SnO₂) nanorods was obtained via annealing a nanoscale precursor in the molten salt flux and surfactant. X-ray diffraction, transmission electron microscopy, high-resolution transmission electron microscopy, selected area electron diffraction and infrared spectroscopy showed that the nanorods are composed of SnO₂ with rutile structure. The surfactant and temperature have a profound influence on the production of SnO₂ nanorods.     

Pulsed-laser-deposited epitaxial aluminum nitride films on (111) Si for surface acoustic-wave applications

Epitaxial (001) aluminum nitride (AlN) thin films on (111) Si substrates are prepared using pulsed-laser deposition. The epitaxial structure of the as-prepared thin films is characterized by checking the X-ray-diffraction θ-2 θ scan and pole-figure, using scanning electron microscopy, infrared radiation (IR) spectroscopy and Raman spectroscopy. The surface acoustic-wave resonance at 345 MHz for a 1.5 μm thick AlN film on a (111) Si substrate is observed using an inter-digital electrode. Received: 18 September 2001 / Accepted: 29 January 2002 / Published online: 3 June 2002 RID="*" ID="*"Corresponding author. Fax: +86-25/359-5535, E-mail: liujm@nju.edu.cn     

Synthesis, morphologies and Raman-scattering spectra of crystalline stannic oxide nanowires

SnO₂ nanowires were synthesized using a direct gas reaction route and were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), selected-area electron diffraction (SAED), high-resolution transmission electron microscopy (HRTEM) and Raman-scattering spectroscopy. XRD, SEM, SAED and HRTEM indicated that the products were tetragonal SnO₂ nanowires with diameters of 10–50 nm. The nanowires were single crystal and solid inside. Dendritic nanowires were observed for the first time. Three vibrational modes were observed in the Raman spectra of the samples. Received: 7 January 2002 / Accepted: 11 April 2002 / Published online: 19 July 2002