Large-scale synthesis of In2O3 nanowires

In₂O₃ nanowires have been successfully fabricated on a large scale from indium particles by thermal evaporation at 1030 °C. The as-synthesized products were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). SEM and TEM images show that these nanowires are uniform with diameters of about 60–120 nm and lengths of about 15–25 μm. XRD and selected-area electron diffraction analysis together indicate that these In₂O₃ nanowires crystallize in a cubic structure of the bixbyite Mn₂O₃ (I) type (also called the C-type rare-earth oxide structure). The growth mechanism of these nanowires is also discussed. Received: 29 June 2001 / Accepted: 28 September 2001 / Published online: 20 December 2001     

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     

Large-scale synthesis of GaN nanorods and their photoluminescence

Large quantities of gallium nitride (GaN) nanorods have been synthesized via direct reaction of metallic gallium vapor with flowing ammonia at 970 °C in a quartz tube. The nanorods have been confirmed as crystalline wurzite GaN by powder X-ray diffraction, selected-area electron diffraction and X-ray photoelectron spectrometry. Transmission electron microscopy and scanning electron microscopy reveal that the nanorods are straight and uniform, with diameters ranging from 40 nm to 150 nm and lengths up to hundreds of micrometers. The growth mechanism is discussed briefly. Photoluminescence measurements on bulk GaN nanorods at room temperature show two strong peaks at 377 nm (3.28 eV) and 360 nm (3.44 eV) attributed to the zero-phonon donor-acceptor pair transition and the donor-bound exciton, respectively. Received: 19 April 2001 / Accepted: 10 May 2001 / Published online: 20 June 2001     

Micrometer-sized Si-Sn-O novel structures with SiONWs on their surfaces

Novel micrometer-sized Si-Sn-O structures with SiO₂ nanowires (SiONWs) growing from their surfaces have been achieved at about 980 °C on Si (111) wafer catalyzed by Sn vapor generated from Sn powders. The Si wafer itself served as a silicon source in the reaction. The micrometer-sized structures, with diameters of several micrometers to several tens of micrometers consisted of Sn, Si and O. The amorphous SiONWs growing from the surface of the micrometer-sized structures were smooth, with diameters about 120 nm and with a composition close to that of SiO₂. The growth mechanism of these novel structures is discussed briefly. Received: 30 July 2002 / Accepted: 18 September 2002 / Published online: 4 December 2002 RID="*" ID="*"Corresponding author. Fax: +86-551/5591434, E-mail: shsuncn@hotmail.com     

Ion synthesis and laser annealing of Cu nanoparticles in Al2O3

Al₂O₃ samples with Cu nanoparticles, synthesised by ion implantation at 40 keV with a dose of 1×10¹⁷ ion/cm² and a current density from 2.5 to 12.5 μA/cm², were annealed using ten pulses from a KrF excimer laser with a single pulse fluence of 0.3 J/cm². The copper depth distribution, formation and modification of metal nanoparticles under the ion implantation and laser treatment were studied by Rutherford backscattering (RBS), energy dispersive X-ray (EDX) analysis, atomic force microscopy (AFM) and optical spectroscopy. It was found that laser annealing leads to a reduction in the nanoparticle size without diffusion of metal atoms into the bulk. The change in particle size and the possibility for oxidation of the copper particles are examined in the framework of Mie theory. Calculations presented show that under excimer laser treatment, Cu nanoparticles are more likely to be reduced in size than to undergo oxidation. Received: 19 April 2001 / Accepted: 7 November 2001 / Published online: 23 January 2002     

Strong green luminescence of Ni2+-doped ZnS nanocrystals

ZnS nanoparticles doped with Ni²⁺ have been obtained by chemical co-precipitation from homogeneous solutions of zinc and nickel salt compounds, with S^2- as precipitating anion, formed by decomposition of thioacetamide (TAA). The average size of particles doped with different mole ratios, estimated from the Debye–Scherrer formula, is about 2–2.5 nm. The nanoparticles could be doped with nickel during synthesis without altering the X-ray diffraction pattern. A Hitachi M-850 fluorescence spectrophotometer reveals the emission spectra of samples. The absorption spectra show that the excitation spectra of Ni-doped ZnS nanocrystallites are almost the same as those of pure ZnS nanocrystallites (λ_ex=308–310 nm). Because a Ni²⁺ luminescent center is formed in ZnS nanocrystallites, the photoluminescence intensity increases with the amount of ZnS nanoparticles doped with Ni²⁺. Stronger and stable green-light emission (520 nm) (its intensity is about two times that of pure ZnS nanoparticles) has been observed from ZnS nanoparticles doped with Ni²⁺. Received: 18 December 2000 / Accepted: 17 March 2001 / Published online: 20 June 2001     

Synthesis and photoluminescence of aligned SiO<Subscript>x</Subscript> nanowire arrays

Aligned SiO_x nanowire arrays standing on a Si substrate were successfully synthesized using a simple method by heating a single-crystalline Si slice covered with SiO₂ nanoparticles at 1000 °C in a flowing Ar atmosphere. The SiO_x nanowire arrays were characterized by scanning electron microscopy and transmission electron microscopy. The SiO_x nanowires become progressively thinner from bottom to top. The formation process of the SiO_x nanowire arrays is closely related to a vapor–solid mechanism. Room-temperature photoluminescence measurements under excitation at 260 nm showed that the SiO_x nanowire arrays had a strong blue–green emission at 500 nm (about 2.5 eV), which may be related to oxygen defects. Received: 29 April 2002 / Accepted: 30 April 2002 / Published online: 10 September 2002 RID="*" ID="*"Corresponding author. Fax: +86-551-559-1434, E-mail: gwmeng@mail.issp.ac.cn     

Template synthesis of single-crystal Cu nanowire arrays by electrodeposition

Cu nanowire arrays have been synthesized using potentiostatic electrodeposition within the confined nanochannels of a porous anodic alumina membrane. The Cu nanowire arrays and the individual nanowires have been characterized using SEM, TEM, SAED, HREM and XRD. Investigation results reveal that the Cu nanowire arrays having high wire packing densities are highly ordered over large areas. The individual Cu nanowires (diameter ∼60 nm) were single-crystal and found to be dense and continuous with uniform diameters throughout their entire length. An optimum ECD condition (at lower overpotentials) for the synthesis of single-crystal Cu nanowires was also discussed. Received: 19 April 2001 / Accepted: 28 April 2001 / Published online: 20 June 2001     

Porous ZnO nanobelts evolved from layered basic zinc acetate nanobelts

Novel porous ZnO nanobelts were successfully synthesized by heating layered basic zinc acetate (LBZA) nanobelts in the air. The precursor of LBZA nanobelts consisted of a lamellar structure with two interlayer distances of 1.325 and 0.99 nm were prepared using a low-temperature, solution-based method. X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and infrared spectroscopy are used to characterize the as-products. PL measurements show that the porous ZnO nanobelts have strong ultraviolet emission properties at 380 nm, while no defect-related visible emission is detected. The good performance for photoluminescence emission makes the porous ZnO nanobelts promising candidates for photonic and electronic device applications.     

Catalytic synthesis of single-crystalline gallium nitride nanobelts

Single-crystalline gallium nitride nanobelts have been synthesized through the reaction of gallium vapor with flowing ammonia using nickel as a catalyst. The as-synthesized products were characterized using X-ray powder diffraction (XRD), scanning electron microscopy, energy-dispersive X-ray spectroscopy, transmission electron microscopy, and selected-area electron diffraction (SAED). XRD and SAED results revealed that the products are pure, single-crystalline GaN with hexagonal structure. The widths and thickness of the nanobelts ranged from 80 to 200 nm, and 10 to 30 nm, respectively. The lengths were up to several tens of micrometers. The nanobelts had smooth surface with no amorphous sheath, and a sharp-tip end. The growth mechanism of nanobelts was discussed.     

Photoluminescence characteristics of ZnS nanocrystallites doped with Ti3+and Ti4+

Direct synthesis of ZnS nanocrystallites doped with Ti³⁺ or Ti⁴⁺ by precipitation has led to novel photoluminescence properties. Detailed X-ray diffraction (XRD), fluorescence spectrophotometry, UV–vis spectrophotometry and X-ray photoelectron spectroscopy (XPS) analysis reveal the crystal lattice structure, average size, emission spectra, absorption spectra and composition. The average crystallite size doped with different mole ratios, estimated from the Debye–Scherrer formula, is about 2.6±0.2 nm. The nanoparticles can be doped with Ti³⁺ and Ti⁴⁺ during the synthesis without the X-ray diffraction pattern being altered. The strong and stable visible-light emission has been observed from ZnS nanocrystallites doped with Ti³⁺ (its maximum fluorescence intensity is about twice that of undoped ZnS nanoparticles). However, the fluorescence intensity of the ZnS nanocrystallites doped with Ti⁴⁺ is almost the same as that of the undoped ZnS nanoparticles. The emission peak of the undoped sample is at 440–450 nm. The emission spectrum of the doped sample consists of two emission peaks, one at 420–430 nm and the other at 510 nm. Received: 27 April 2001 / Accepted: 16 August 2001 / Published online: 17 October 2001     

Synthesis and photoluminescence characteristics of doped ZnS nanoparticles

Free-standing powders of doped ZnS nanoparticles have been synthesized by using a chemical co-precipitation of Zn²⁺, Mn²⁺, Cu²⁺ and Cd²⁺ with sulfur ions in aqueous solution. X-ray diffraction analysis shows that the diameter of the particles is ∼2–3 nm. The unique luminescence properties, such as the strength (its intensity is about 12 times that of ZnS nanoparticles) and stability of the visible-light emission, were observed from ZnS nanoparticles co-doped with Cu²⁺ and Mn²⁺. The nanoparticles could be doped with copper and manganese during the synthesis without altering the X-ray diffraction pattern. However, doping shifts the luminescence to 520–540 nm in the case of co-doping with Cu²⁺ and Mn²⁺. Doping also results in a blue shift on the excitation wavelength. In Cd²⁺-doped ZnS nanometer-scale particles, the fluorescence spectra show a red shift in the emission wavelength (ranging from 450 nm to 620 nm). Also a relatively broad emission (ranging from blue to yellow) has been observed. The results strongly suggest that doped ZnS nanocrystals, especially two kinds of transition metal-activated ZnS nanoparticles, form a new class of luminescent materials. Received: 16 October 2000 / Accepted: 17 October 2000 / Published online: 23 May 2001     

Luminescence from copper nanoparticles

The presence of copper nanoparticles in alumina and silica modifies their luminescence, and the changes in spectra are influenced by variations in the nanoparticle size distributions. Luminescence signals are sensitive to the total defect population. Thus the luminescence not only reflects changes caused by thermal annealing, which can modify both intrinsic defects and the copper nanoparticles, but also responds to the method of preparation of thin film layers. Copper nanoparticle influence on luminescence is reported both for ion-implanted bulk silica and for copper in pulsed laser deposition within alumina. Luminescence thus potentially offers a non-destructive monitor of the layer quality, reproducibility and growth conditions, as well as the state and size of the copper nanoparticles. Received: 29 June 2001 / Published online: 10 October 2001     

Template synthesis of Y-junction metal nanowires

Template synthesis of large-scale Y-junction metal nanowires is reported. In this approach, a Y-shaped nanochannel porous anodic alumina (PAA) template is prepared by using a two-step anodization of aluminum in which the metal of interest, such as copper, is electrodeposited to form the Y-junction metal nanowires. The synthesis method presented here is simple and versatile. This method can be extended to the preparation of other Y-junction nanowires with desirable composition and shows great promise for the development of nanoelectronics. Received: 10 September 2001 / Accepted: 20 November 2001 / Published online: 23 January 2002     

Fabrication and characterization of In2O3 nanowires

In₂O₃ nanowires were successfully fabricated through a simple gas-reaction route in argon atmosphere. These nanowires have diameters ranging from 20 nm to 50 nm and lengths up to tens of micrometers. High-resolution transmission electron microscopy observations and the electron-diffraction (ED) pattern reveal that the In₂O₃ nanowires are formed by the stacking of (2) planes along the [1] direction, which is parallel to the wire axis. A strong and wide ultraviolet (UV) emission band centered at around 392 nm is observed for the first time in the room-temperature photoluminescence measurement in addition to the usual blue emission (468 nm). Moreover, five discrete fine peaks (372 nm, 383 nm, 406 nm, 392 nm and 413 nm) are further identified in this broad UV band. Received: 10 April 2002 / Accepted: 12 April 2002 / Published online: 19 July 2002     

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     

New synthesis of multi-walled carbon nanotubes using an arc discharge technique under organic molecular atmospheres

We have synthesized multi-walled carbon nanotubes (MWNTs) using a DC arc discharge method under organic molecular atmospheres. This method allows us to synthesize about five times more MWNTs than are synthesized using the usual arc discharge method, using discharge conditions of 100 A and 20 V. We have examined the synthetic yield of MWNTs at various pressures under different organic atmospheres. The yield of MWNTs increases with the number of carbon atoms in the organic molecule. Received: 21 September 2000 / Accepted: 18 December 2000 / Published online: 26 April 2001     

Size distributions and synthesis of nanoparticles by photolytic dissociation of ferrocene

Iron-containing nanoparticles were made by laser-assisted (ArF excimer laser, λ=193 nm) photolytic dissociation of ferrocene (Fe(C₅H₅)₂ or FeCp₂) in argon and an oxygen/argon gas mixture. The particle-size distributions were obtained on-line by using differential mobility analysers (DMAs) and were found to be log-normal with a geometric standard deviation of 1.85. In argon, particle sizes between 3 and 100 nm were generated. The volumes of these particles were found to increase linearly with the increased repetition rate, fluence and beam size of the laser. These observations are explained on the basis of the residence-time approach model. Received: 23 November 1999 / Accepted: 19 September 2000 / Published online: 22 November 2000     

Morphologies of GaN one-dimensional materials

GaN one-dimensional materials with different morphologies were formed on LaAlO₃ crystal, silicon crystal and quartz glass substrates through a simple sublimation method. They were characterized by powder X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and energy-dispersive X-ray (EDX) spectroscopy. FE-SEM images showed that the morphologies of the one-dimensional materials included straight nanorods, curved nanowires, nanoribbons, zigzag nanorods and beaded or capture-tree nanorods. XRD and EDX studies indicated that all the one-dimensional materials were wurtzite GaN. Received: 14 July 2000 / Accepted: 17 July 2000 / Published online: 20 September 2000     

Synthesis of aligned gallium nitride nanowire quasi-arrays

Self-aligned GaN nanowire quasi-arrays were synthesized on MgO crystal through a simple gas reaction method. They were characterized by powder X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray (EDX) spectroscopy and high-resolution transmission electron microscopy (HRTEM). FE-SEMimages showed that the product consisted of quasi-arrays of nanowires. XRD, EDX and HRTEM indicated that the nanowires were wurtzite GaN single crystals. Received: 19 June 2000 / Accepted: 21 June 2000 / Published online: 9 August 2000