Size-controlled synthesis and gas sensing application of tungsten oxide nanostructures produced by arc discharge.

Several different synthetic methods have been developed to fabricate tungsten oxide (WO(3)) nanostructures, but most of them require exotic reagents or are unsuitable for mass production. In this paper, we present a systematic investigation demonstrating that arc discharge is a fast and inexpensive synthesis method which can be used to produce high quality tungsten oxide nanostructures for NO(2) gas sensing measurements. The as-synthesized WO(3) nanostructures are characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), finger-print Raman spectroscopy and proton induced x-ray emission (PIXE). The analysis shows that spheroidal-shaped monoclinic WO(3) crystal nanostructures were produced with an average diameter of 30 nm (range 10-100 nm) at an arc discharge current of 110 A and 300 Torr oxygen partial pressure. It is found that the morphology is controlled by the arc discharge parameters of current and oxygen partial pressure, e.g. a high arc discharge current combined with a low oxygen partial pressure results in small WO(3) nanostructures with improved conductivity. Sensors produced from the WO(3) nanostructures show a strong response to NO(2) gas at 325 °C. The ability to tune the morphology of the WO(3) nanostructures makes this method ideal for the fabrication of gas sensing materials.

Fabrication of surface magnetic nanoclusters using low energy ion implantation and electron beam annealing.

Magnetic nanoclusters have novel applications as magnetic sensors, spintronic and biomedical devices, as well as applications in more traditional materials such as high-density magnetic storage media and high performance permanent magnets. We describe a new synthesis protocol which combines the advantages of ion implantation and electron beam annealing (EBA) to produce surface iron nanoclusters. We compare the structure, composition and magnetic properties of iron nanoclusters fabricated by low dose 15 keV Fe implantation into SiO(2) followed by 1000 °C EBA or furnace annealing. Atomic force microscopy (AFM) and high resolution transmission electron microscopy (HRTEM) images together with superconducting quantum interference device (SQUID) magnetometry measurements show that only EBA leads to the rapid formation of surface crystalline Fe spherical nanoclusters, showing magnetic moments per Fe atom comparable to that of bulk bcc Fe and superparamagnetic properties. We propose a fabrication mechanism which includes e-beam enhanced desorption of SiO(2). This method has potential for fabricating nanoscale magnetic sensors integrated in microelectronic devices.

Modulation of field emission properties of znO nanorods during arc discharge.

Zinc oxide (ZnO) nanorods have been synthesized via the arc discharge method. Different oxygen partial pressures were applied in the arc discharge chamber to modulate the field emission properties of the as-synthesized ZnO nanorods. Scanning electron microscopy (SEM) was carried out to analyze the morphology of the ZnO nanorods. The ion beam analysis technique of proton induced X-ray emission (PIXE) was performed to probe the impurities in ZnO nanorods. SEM images clearly revealed the formation of randomly oriented ZnO nanorods with diameters between 10-50 nm. It was found that the morphology and the electrical properties of the ZnO nanorods were dependent on the oxygen partial pressure during arc discharge. In addition enhanced UV-sensitive photoconductivity was found for ZnO nanorods synthesized at high oxygen partial pressure during arc discharge. The field emission properties of the nanorods were studied. The turn-on field, which is defined at a current density of 10 microA cm(-2), was about 3 V microm(-1) for ZnO nanorods synthesized at 99% oxygen partial pressure during arc discharge. The turn-on field for ZnO nanorods increased with the decrease of oxygen partial pressure during arc discharge. The simplicity of the synthesis route coupled with the modulation of field emission properties due to the arc discharge method make the ZnO nanorods a promising candidate for a low cost and compact cold cathode material.

Electron beam annealing of Fe+ implanted Si nanostructures.

Silicon nanostructures (nanowhiskers) have been formed at surface densities approximately 10(9) cm-2 by electron beam annealing (EBA) prior to the implantation of 7 keV Fe+ ions to fluences from 1 x 10(13) - 4 x 10(15) Fe+ cm(-2). A second EBA step is then applied to relieve implantation-induced stresses. RBS analysis shows that the implanted Fe remains close to the surface. AFM characterisations of the implanted nanowhiskers before and after the final EBA step are summarised in graphs of height versus surface density. In a striking result it is shown that the nanowhiskers not only survive processing but also grow significantly. For example, at the highest fluence of 4 x 10(15) Fe+ cm(-2), the average height more than doubles: the increases are from 5.0 nm to 6.5 nm under implantation and from 6.5 nm to 11.8 nm under EBA. In addition there is a significant increase in surface density from an initial value of 1.6 x 10(9) cm(-2) to 4.3 x 10(9) cm(-2). These results highlight the feasibility of doping Si surface nanostructures with magnetic ions to fabricate Si devices for spin-dependent enhanced field emission.

Ordered array of self-assembled SiC nanocrystals fabricated by selective oxide desorption and nanosphere lithography.

We have developed a novel technique based on the selective desorption of an oxide film in order to grow ordered arrays of silicon carbide nanocrystals on a silicon surface. These nanocrystals form as a byproduct of void nucleation in the oxide during the high-temperature vacuum annealing of silicon, a process which normally produces a random distribution of nanocrystals across the silicon surface after its oxide layer has been fully desorbed. By the pre-deposition of a thin layer of excess silicon on the oxide surface through a patterned lithography mask, site-specific nucleation of voids in the silicon oxide can instead be achieved during the annealing step, leading to the growth of silicon carbide nanocrystals in regular patterns over the silicon surface.

UV and humidity sensing properties of ZnO nanorods prepared by the arc discharge method.

The UV and humidity sensing properties of ZnO nanorods prepared by arc discharge have been studied. Scanning electron microscopy and photoluminescence spectroscopy were carried out to analyze the morphology and optical properties of the as-synthesized ZnO nanorods. Proton induced x-ray emission was used to probe the impurities in the ZnO nanorods. A large quantity of high purity ZnO nanorod structures were obtained with lengths of 0.5-1 microm. The diameters of the as-synthesized ZnO nanorods were found to be between 40 and 400 nm. The nanorods interlace with each other, forming 3D networks which make them suitable for sensing application. The addition of a polymeric film-forming agent (BASF LUVISKOL VA 64) improved the conductivity, as it facilitates the construction of conducting networks. Ultrasonication helped to separate the ZnO nanorods and disperse them evenly through the polymeric agent. Improved photoconductivity was measured for a ZnO nanorod sensor annealed in air at 200 degrees C for 30 min. The ZnO nanorod sensors showed a UV-sensitive photoconduction, where the photocurrent increased by nearly four orders of magnitude from 2.7 x 10(-10) to 1.0 x 10(-6) A at 18 V under 340 nm UV illumination. High humidity sensitivity and good stability were also measured. The resistance of the ZnO nanorod sensor decreased almost linearly with increasing relative humidity (RH). The resistance of the ZnO nanorods changed by approximately five orders of magnitude from 4.35 x 10(11) Omega in dry air (7% RH) to about 4.95 x 10(6) Omega in 95% RH air. It is experimentally demonstrated that ZnO nanorods obtained by the arc discharge method show excellent performance and promise for applications in both UV and humidity sensors.

Onset temperature for Si nanostructure growth on Si substrate during high vacuum electron beam annealing.

Silicon nanostructures, called Si nanowhiskers, are successfully synthesized on Si(100) substrate by high vacuum electron beam annealing. The onset temperature and duration needed for the Si nanowhiskers to grow was investigated. It was found that the onset and growth morphology of Si nanowhiskers strongly depend on the annealing temperature and duration applied in the annealing cycle. The onset temperature for nanowhisker growth was determined as 680 degrees C using an annealing duration of 90 min and temperature ramps of +5 degrees C s(-1) for heating and -100 degrees C s(-1) for cooling. Decreasing the annealing time at peak temperature to 5 min required an increase in peak temperature to 800 degrees C to initiate the nanowhisker growth. At 900 degrees C the duration for annealing at peak temperature can be set to 0 s to grow silicon nanowhiskers. A correlation was found between the variation in annealing temperature and duration and the nanowhisker height and density. Annealing at 900 degrees C for 0 s, only 2-3 nanowhiskers (average height 2.4 nm) grow on a surface area of 5 x 5 microm, whereas more than 500 nanowhiskers with an important average height of 4.6 nm for field emission applications grow on the same surface area for a sample annealed at 970 degrees C for 0 s. Selected results are presented showing the possibility of controlling the density and height of Si nanowhisker growth for field emission applications by applying different annealing temperature and duration.

Overstoichiometric low-energy nitrogen implantations into silicon--formation of gas nanobubbles vs. silicon nanowhiskers.

Accelerator-based ion implantation can be used to produce stoichiometric ratios beyond thermodynamic equilibrium. In the studies reported here, single crystalline silicon wafer material was implanted with high fluences of nitrogen. The implantations, performed with 15N at 5 keV/ion, resulted in the formation of highly swollen nitrogen rich surfaces that incorporated up to 63 at.% nitrogen. The implanted specimens were subsequently annealed with electron beams at high temperature, typically 1150 degrees C for moderately short periods of time (15 s) to investigate the formation of silicon nanowhiskers. However, it was observed that nanowhiskers, the formation of which can be expected by comparable understoichiometric implantations, did not appear. Although the shallow implantations created ultrathin silicon nitride films with typical thickness of 25 nm, laterally swollen areas of 400 +/- 50 nm were observed with atomic force microscopy operated in supersonic mode.

Combined NRA, channeling-RBS and FTIR ellipsometry analyses for the determination of the interface and bonding state of thin SiO(x) and SiN(x)O(y) layers.

The molecular ions O(+)(2) and NO(+) are im- planted at room temperature into single-crystal silicon with an energy of E=6 keV/atom at fluences ranging from 2.5x10(16) to 3.5x10(17) at/cm(2). The samples are processed by electron beam rapid thermal annealing at 1100 ( degrees )C for 15 s. The depth distributions of the implanted specimens ((18)O) are determined by nuclear reaction analyses using the reaction (18)O(p,alpha)(15)N. Channeling-RBS measurements are performed to obtain the interface structure between the implanted layer and the single-crystal Si substrate. The chemical bonding state of as-implanted and implanted-annealed specimens is observed by FTIR ellipsometry measurements.