Size and density control of silicon oxide nanowires by rapid thermal annealing and their growth mechanism

In this work, we demonstrate a fast approach to grow SiO₂ nanowires by rapid thermal annealing (RTA). The material characteristics of SiO₂ nanowires are investigated by field emission scanning electron microscopy, high-resolution transmission electron microscopy (HRTEM), high-angle annular dark-field (HAADF) imaging, electron energy loss spectroscopy (EELS), and energy-filtered TEM (EFTEM). The HAADF images show that the wire tip is predominantly composed of Pt with brighter contrast, while the elemental mappings in EFTEM and EELS spectra reveal that the wire consists of Si and O elements. The SiO₂ nanowires are amorphous with featureless contrast in HRTEM images after RTA at 900°C. Furthermore, the nanowire length and diameter are found to be dependent on the initial Pt film thickness. It is suggested that a high SiO₂ growth rate of >1 μm/min can be achieved by RTA, showing a promising way to enable large-area fabrication of nanowires.     

Thermal stability of catalytically grown multi-walled carbon nanotubes observed in transmission electron microscopy

The thermal stability of multi-walled carbon nanotubes (MWCNTs) was assessed in situ by transmission electron microscopy. Upon heating, Ni catalysts in MWCNTs containing bamboo structures shrank from the tail due to evaporation, leading to additional bamboo formation and tube elongation at 800°C, while the MWCNTs with FeSi catalysts remained intact up to 1050°C except for better crystallinity. The physisorbed carbon and/or hydrocarbon on surfaces and super-saturated carbon in the Ni catalysts should be responsible for the phenomena.     

Inorganic WS<Subscript>2</Subscript> nanotubes revealed atom by atom using ultra-high-resolution transmission electron microscopy

The characterization of nanostructures to the atomic dimensions becomes more important, as devices based on a single particle are being produced. In particular, inorganic nanotubes were shown to host interesting properties making them excellent candidates for various devices. The WS₂ nanotubes outperform the bulk in their mechanical properties offering numerous applications especially as part of high strength nanocomposites. In contrast, their electrical properties are less remarkable. The structure–function relationship can be investigated by aberration-corrected high-resolution transmission electron microscopy (HRTEM), which enables the insight into their atomic structure as well as performing spectroscopic measurements down to the atomic scale. In the present work, the deciphering of atomic structure and the chiral angle of the different shells in a multiwall WS2 nanotube is demonstrated. In certain cases, the helicity of the structure can also be deduced. Finally, first electron energy loss spectra (EELS) of a single tube are presented, acquired by a new acquisition technique that allows for high spatial resolution (denoted StripeSTEM). The measured band gap values correspond with the values found in literature for thin films, obtained by spectroscopic techniques, and are higher than the values resulting from STM measurements.     

Observations of nanoscopic,face centered cubic Ti and TiH<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>

Transmission electron microscopy has been used to study ball milled and H cycled NaAlH₄ with 10 mol% TiCl₃. Isolated from the main phases in this hydrogen storage system, nanocrystalline aggregates of fcc TiH _x (0≤x<0.67) were found. The value of x was determined based on the assumption of a linear increase of the TiH _x lattice parameter by increasing H content. The size of the TiH _x crystallites was in the range 10 to 20 nm, and the lattice parameter decreased from 4.22 Å in TiH_0.67 to 4.10 Å in pure fcc Ti. Non-equilibrium ball milling and subsequent H cycling in combination with a small crystallite size are believed to make the TiH _x phase stable. The present results are the first observations of fcc TiH _x with low hydrogen content, and the measured fcc lattice parameter of Ti matches first-principles calculations.     

Imaging and spectroscopy of defects in semiconductors using aberration-corrected STEM

The distribution of single dopant or impurity atoms can dramatically alter the properties of semiconductor materials. The sensitivity to detect and localize such single atoms has been greatly improved by the development of aberration correctors for scanning transmission electron microscopes. Today, electron probes with diameters well below 1 Å are available thanks to the improved electron optics. Simultaneous acquisition of image signals and electron energy-loss spectroscopy data provides means of characterization of defect structures in semiconductors with unprecedented detail. In addition to an improvement of the lateral spatial resolution, depth sensitivity is greatly enhanced because of the availability of larger probe forming angles. We report the characterization of an alternate gate dielectric interface structure. Isolated Hf atoms are directly imaged within a SiO₂ thin film formed between an HfO₂ layer and the silicon substrate. Electron energy-loss spectroscopy shows significant changes of the silicon valence state across the interface structure.     

Temperature dependence of photoconductivity and persistent photoconductivity of single ZnO nanowires

Photoelectrical properties of single ZnO nanowires have been investigated using photocurrent–voltage characteristics measurements varying with excitation photon energy and temperature. It is found that persistent photoconductivity (PPC) exists, and the PPC decreases with decreasing temperature. The temperature dependence of the PPC effect indicates that thermally activated return of electrons from shallow traps is responsible for the PPC phenomenon. The photosensitivity is found to be linear with the applied voltage, and it increases with decreasing temperature. A temperature dependence of photoconductivity gain was introduced to explain the experimental results.     

Synthesis of ZnO hollow spherical structures with different surface-to-volume ratios

ZnO hollow spherical structures with different surface-to-volume ratios were prepared using solid Zn microspheres as template via a simple oxygen-controlled thermal evaporation approach. The results of scanning electron microscopy testify that ZnO hollow spherical structures with different morphologies can be realized by changing oxygen supply. The corresponding transmission electron microscopy images further reveal that the prepared spherical structures are hollow, and nanorods epitaxially grow from the surface of the sphere shell along the [0001] direction. A series of experiments indicates that the formation of hollow spherical structures involves the oxidization on the surface of Zn microspheres, sublimation of Zn, and growth of ZnO nanorods.     

Highly oriented electrospun polycaprolactone micro/nanofibers prepared by a field-controllable electrode and rotating collector

Novel ZnO tetrapod-shaped nanostructures with pearl-necklace-shaped arms were successfully synthesized using mixture of Zn, ZnO, and carbon powder as source. The definite supersaturation ratio provided by Zn, ZnO, and carbon powder was considered as the crucial factor of determining the formation of this kind of structure, and a negative feedback growth model combined with octahedral nucleation mechanism was proposed. Two other comparative experiments were also conducted to study the growth behavior of reagent species under different supersaturation ratios. Our experiments provided a beneficial experimental exploration in controlled growth of nanostructures through modulating supersaturation ratio by source, and these obtained novel nanostructures were also expected to have potential application as functional blocks in nanodevices. Furthermore, the study of photoluminescence indicated that the physical properties were strongly dependent on the crystal structure.     

TiO<Subscript>2</Subscript> microstructures by inversion of macroporous silicon using atomic layer deposition

An approach is presented which is capable of fabricating arbitrarily shaped three-dimensional microstructures. Two methods—namely, macroporous silicon and atomic layer deposition—are combined to realize structures in the micrometer and submicrometer range. Using TiO₂ as an example, the fabrication of single hollow objects as well as complex network structures is shown. The scalability and the wide range of applicable materials are the key points of this method for future applications.     

Evidences dominating the formation of ZnO nanostructures via in-situ study in an environmental scanning electron microscope

In order to well understand the growth mechanism of the diverse morphology of the ZnO nanostructures, in situ analysis of the formation of different ZnO nanostructures, such as nanowires, nanocombs, and nanosheets, has been conducted in an environmental scanning electron microscope (ESEM). It is found that both nanocombs and nanosheets grew in two-stage heating processes on parent nanowires. The difference is that the nanocombs were synthesized in extremely high pressure of zinc vapor via a self-catalyzed vapor-liquid-solid process, while the ZnO nanosheets were grown in relatively low pressure of zinc vapor. All the growth processes were revealed in real time imaging. It is demonstrated that the change in the growth environments can influence the thickness of the ZnO polycrystalline surface of the zinc powder, which alters the pressure of the zinc vapor and in turn determines the morphology of the final nanostructures.     

Growth and characterization of oriented CdSe nanobelts and nanorods

Oriented CdSe nanobelts and nanorods were grown successfully on GaAs and Si substrates by metal organic chemical vapor deposition. The thickness of Au film coated on the substrate plays an important role in determining the orientation, size, and density of these one-dimensional CdSe nanostructures. Preferred orientation was observed for nanostructures grown on the GaAs substrate coated with thick Au film, but not for the nanostructures grown on the Si substrate. Photoluminescence, transmission electron microscope, and X-ray diffraction measurements show that the CdSe nanostructures could have either wurtzite or zinc-blende structures, and there are more nanostructures with wurtzite structure than with zinc-blende structure.     

Fabrication of completely filled carbon nanotubes with copper nanowires in a confined space

Carbon nanotubes (CNTs) filled completely with polycrystalline Cu nanowires were synthesized by laser vaporization of Cu and graphite under high-pressure Ar gas atmosphere. Depending on the Ar gas pressure (0.1–0.9 MPa) and the Cu content (1–40 at.%) in graphite targets for laser vaporization, various products with different morphologies were observed by scanning and transmission electron microscopy. The ratios of the Cu-filled CNTs and carbon nanocapsules particularly increased as Ar gas pressure was increased. The maximum ∼60% fraction of Cu-filled CNTs with outer diameter of 10–50 nm and length of 0.3–3 μm was achieved at 0.9 MPa from graphite containing 20 at.% Cu. Most of the encapsulated Cu-nanowires were surrounded by single, double, or triple graphitic layers. Although the yield of the Cu-filled CNTs was also dependent on the Cu content in the graphite targets, no unfilled CNTs were produced even for low Cu content. The growth of Cu-filled CNTs is explained by the formation of molten Cu–C composite particles with an unusually C-rich composition in a space confined by high-pressure Ar gas, followed by precipitating Cu and C from the particles and subjecting them to phase separation.     

The effects of chemical etching of porous silicon on Raman spectra

We have investigated the effects of chemical etching on Raman spectra of porous silicon. The as-anodized porous silicon consisted mainly of crystalline silicon, as indicated by the Raman spectra. The background in the spectrum was strong, indicating that the porous silicon surface was rough due to the presence of pores. When chemical etching was performed five times, the Raman spectrum revealed the presence of spherically shaped nanocrystalline silicon whose diameter was around 3.5 nm. Further chemical etching, however, extinguished the nanocrystallites, in addition to smoothing the surface morphology.     

Polycrystalline silicon films obtained by hot-wire chemical vapour deposition

Silicon films were deposited at moderate substrate temperatures (280–500° C) from pure silane and a silane-hydrogen mixture (10% SiH₄, 90% H₂) in a hotwire CVD reactor. The morphology, structure and composition of the samples were studied with scanning electron microscopy, transmission electron microscopy, transmission electron diffraction, X-ray diffraction, Raman spectroscopy and secondary ion mass spectrometry. The sample deposited at 500° C with pure silane has an amorphous structure, whereas the samples obtained from silane diluted in hydrogen have a polycrystalline structure, even that grown at the lowest temperature (280° C). Polycrystalline samples have a columnar structure with 0.3–1 m crystallite sizes with preferential orientation in [220] direction. Deposition rates depend on the filament-substrate distance and range from 9.5 to 37 Å/s for the polycrystalline samples. The high quality of the polycrystalline samples obtained makes the hot-wire technique very promising. Moreover, it is expected to be easily scaled up for applications to large-area optoelectronic devices and to photovoltaic solar cells.     

Isotopic dependence of electron screening in fusion reactions

The fusion reactions⁶Li(p, )³He,⁶Li(d, )⁴He, and⁷Li(p, )⁴He have been studied over the c.m. energy rangeE=10 to 1450 keV. Each reaction involved the use of hydrogen projectiles and LiF solid targets as well as Li projectiles and hydrogen molecular gas targets. In all cases the effects of electron screening on the low-energy fusion cross sections (exponential enhancement) have been observed; the effects are somewhat stronger in the case of atomicp ord projectiles compared to the case of molecularH ₂ orD ₂ gas targets. If isotopic effects on electron screening are negligible, all three reactions should exhibit the same enhancements for each set of experimental techniques. The measurements confirmed this expectation to a large extent.Supported in part by the Landesamt Nordrhein-Westfalen (IVA5-10600387), the Deutsche Forschungsgemeinschaft (Ro429/ 18-2 and Ro429/21-1), and the Comision Interministerial de Ciencia y Tecnologia (AEN90-0932)     

Growth mechanism of scales of SiC nanowires with/without ZnS powders at varying temperatures

The growth mechanism of scales of crystalline SiC nanowires (SiC-NWs) obtained by directly evaporating solid carbon on silicon wafer with/without ZnS powders at varying temperatures is being discussed. More aligned SiC-NWs of small size and good crystalline structure were formed when ZnS was used. Random SiC-NWs of big size and poor crystalline structure were obtained at conditions free of ZnS. Furthermore, the improved crystalline structure and increased diameter of SiC-NWs were observed when the higher temperature was employed.     

Nonlinear refraction of silver nanowires from nanosecond to femtosecond laser excitation

In order to investigate the effect of pulse width and solvent on the nonlinear properties of metal nanostructures, silver nanowires were fabricated in a direct current electric field (DCEF) using a solid-state ionic method and characterized by transmission electron microscopy (TEM) and X-ray diffraction (XRD). The nonlinear refractive index (γ) of silver nanowires suspended in ethanol was measured using the Z-scan technique and laser radiation of various (femto-, pico-, and nanosecond) pulse durations. Experimental results indicated that silver nanowires have obvious positive refractive nonlinearities and γ (the Kerr-induced self-focusing) increases as the pulse duration increases from 7.4×10⁻⁸ cm²/GW at 110 fs to 1.6×10⁻⁴ cm²/GW at 8 ns, due to the additional influence of the atomic reorientational Kerr effect in the case of longer pulses. Due to the solvent dependence of the nonlinear behavior of the silver nanowires, the nonlinear absorption and refraction of silver nanowires suspended in de-ionized water are smaller than those of silver samples suspended in ethanol. The thermal nonlinearities are insignificant in our experimental conditions.     

<Emphasis Type="Italic">Para</Emphasis>-hexaphenyl nanofiber growth on Au-coated porous alumina templates

The availability of easy and reproducible methods for formation of periodically nanostructured surfaces allows one to study the quasi-epitaxial growth of nanowires on such artificially modified substrates. Here, we demonstrate that crystalline nanofibers of para-hexaphenyl can grow on porous alumina templates with high pore regularity once the templates have been coated by a thin Au film. Nanofibers of that kind represent a model system for the general class of organic nanowires which have chemically changeable optoelectronic properties and hence are of interest for integration into future optoelectronic devices.     

Structural properties of size-selected FeCo nanoparticles deposited on W(110)

Size-selected iron and iron–cobalt alloy clusters have been studied with high resolution transmission electron microscopy (HRTEM) and scanning tunneling microscopy (STM). The clusters were produced by a continuously working arc cluster ion source and subsequently size-selected by an electrostatic quadrupole deflector. The crystalline structure of pure clusters has been investigated with HRTEM to ensure a reliable determination of the lattice parameter for the alloy clusters. The composition of the alloy clusters was checked with energy dispersive X-ray spectroscopy (EDX). The height of the deposited FeCo clusters on the (110) surface of tungsten was determined via STM. These results were compared with the lateral size distribution being investigated by TEM and allow a conclusion on the shape of the deposited alloy clusters. Furthermore, the behavior of the alloy clusters on the W(110) surface at elevated temperatures has been examined, at which the clusters show anisotropic spreading.     

The use of linear superconducting electron accelerator for subcritical reactor driving

At the National Science Centre, Kharkiv Institute of Physics and Technology (NSC KIPT) the possibility of creating an installation with a subcritical reactor driven by an electron accelerator is examined. To obtain the maximal stream of neutrons from a neutron-producing target at a minimal density of energy emission, the electron energy should be in the range of 100–200 MeV and the size of the target should be as large as possible. Other important requirements are beam continuity with time and long-term stability of the accelerator parameters. The variants of using the superconducting linear accelerator on the basis of a TESLA accelerating structure as of subcritical reactor driver are considered. The basic design parameters and characteristics of this installation are presented. The text was submitted by the authors in English.