Hiroyuki Sakaue

Ordered Two-Dimensional Nanowire Array Formation Using Self-Organized Nanoholes of Anodically Oxidized Aluminum

Self-organization of a two-dimensional array of nanoholes which were formed by anodic oxidation of aluminum was investigated quantitatively using fast Fourier transformation (FFT) analysis of scanning electron microscopy (SEM) images. The highly ordered array of nanoholes with diameters of 26 nm was obtained by two-step anodization at anodic voltage around 40 V, and oxalic acid concentration of 0.5 M. A two-dimensional ordered array of Au free standing nanowires was successfully fabricated by the deposition of Au using DC electroplating in nanoholes of aluminum oxide, by removal of the aluminum oxide barrier layer using wet chemical etching. The present method has a high efficiency to fabricate ordered nanowire array of a variety of conductive materials in a large area, and wide applications for fabricating quantum effect devices and materials would be expected.

Bottom-Up Fill of Copper in Deep Submicrometer Holes by Electroless Plating

Bottom-up fill of Cu in deep submicrometer via holes was achieved through electroless plating alone for the first time. We investigated the effect of addition of inhibitor molecules to electroless Cu plating solution, and found that sulfopropyl sulfonate ~SPS! was highly effective in promoting the bottom-up fill. The tendency for bottom-up filling was enhanced by shrinkage of the hole diameter. This suggests that the diffusion flux of SPS molecules to the bottom of holes was more suppressed for smaller holes.

Digital chemical vapor deposition of SiO2 using a repetitive reaction of triethylsilane/hydrogen and oxidation

The extraction reaction of hydrogen in triethylsilane (TES) with hydrogen radicals generated by a remote plasma of H2 produces an organic Si film. Step coverage features of the film depend strongly on H2 concentration in the TES+H2 reaction system. A conformal profile has been achieved for 60% H2 at 250°C as a result of the low-viscosity nature of the film which includes CxHy groups. With the aim of filling a deep trench with hlgh-quality SiO2 film, digital chemical vapor deposition (CVD), which was carried out by repeating a cycle of the conformal deposition of the Si film and subsequent oxidation, was studied. The SiO2 film which was deposited at 250°C and with an initial thickness per cycle of 5 A at a 1 s oxygen pulse offered a low concentration of organic species, and thus a relatively low BHF etch rate.

Bottom-Up Fill for Submicrometer Copper Via Holes of ULSIs by Electroless Plating

In this report, the hole-filling characteristics upon addition of SPS were evaluated in detail by cross-sectional scanning electron microscopy ~SEM!, and the effects of SPS concentration on bottom-up fill ability, and fundamental film properties such as contaminant level, crystal texture, and surface morphology were investigated. Experimental ICB-Pd layers with a thickness of 1 or 2 nm were deposited on the surface of three types of TaN/SiO2 /Si substrates, hole patterns ~diameter, 0.31-1.0 mm; depth, 1.5 mm! for investigating filling viahole; trench patterns ~length, 100 mm; width, 0.21-100 mm; depth, 0.3 mm! for electrical resistivity measurement; and blankets for measurement of the deposition rate of electroless plating with SPS concentration. The thickness of the Pd layer was determined by a quartz microbalance placed on the substrate surface. Prior to electroless copper plating, all substrates were cleaned by ultrasonication in acetone at room temperature for 10 min. The composition of the electroless copper plating solution was CuSO4 i 5H2O ~6.6 g/L! ,C 10H16N2O8 ~EDTA; 70.0 g/L!, glyoxylic acid ~18.0 g/L! as a reducing agent, 2,28-dipyridine ~0.04 g/L! as stabilizer, polyethylene glycol ~4000 MW, 0.5 g/L! as the surface activator. The pH of the plating bath was adjusted to approximately 12.5 using tetramethylammonium hydroxide ~TMAH! and the bath temperature was maintained at 70°C. The interfacial structure and morphology of samples were characterized by field-emission scanning electron microscopy~FE-SEM! and field-emission transmission electron microscopy~FE-TEM! .A ll SEM and TEM samples were prepared by focused ion beam ~FIB!. To protect the surface of the Cu film for etching during FIB cutting, a fine film of epoxy resin was coated on the surface of Cu by spin

Well-size-controlled Colloidal Gold Nanoparticles Dispersed in Organic Solvents.

The preparation of well-size-controlled colloidal gold nanoparticles in organic solvent is presented. After the preparation of well-size-controlled aqueous colloidal gold particles, we changed the solvent to an organic one. This technique is required to enable a chemical reaction between gold particles and hydrophobic molecules, since a colloidal gold solution is typically prepared in water using a reduction process. We also investigated the stability of the gold particle suspension, and found that the stability decreases in the sequence of water, ethanol, chloroform, and benzene solution.

Experimental conditions for a highly ordered monolayer of gold nanoparticles fabricated by the Langmuir–Blodgett method

A highly ordered monolayer film of alkanethiol-encapsulated gold nanoparticles was fabricated on a silicon substrate by using the Langmuir–Blodgett (LB) method. The effects on the particle order, of the particle concentration and the type of solvent of the LB spreading suspension of encapsulated gold particles, were studied. We found that a low particle concentration of 0.06–0.3 mg/mL in chloroform is optimal for the fabrication of high quality gold particle monolayers. Since the proposed method is not restricted to gold particles, it is believed to be a practical process for fabricating quantum dot structures of various particle sizes and compositions.

Tungsten spectra recorded at the LHD and comparison with calculations

We have measured extreme ultraviolet (EUV) spectra from highly charged tungsten ions in low-density and high-temperature plasmas produced in the Large Helical Device at the National Institute for Fusion Science. The EUV spectra emitted after injection of a tungsten pellet into a hydrogen plasma were recorded at plasma temperatures of 1.5 and 3 keV and were dominated by an intense transition array in the 4.5–6.5 nm region, the profile and extent of which was different in both spectra. Some discrete lines present were identified by comparison with existing spectral data while atomic structure calculations showed that the dominant emission in both arose from Δn = 0, n = 4–n = 4 transitions and the main differences could be attributed to the appearance of the 4p–4d and 4s–4p transitions from W XXXIX to W XLVI in the higher temperature spectrum. Comparison with calculations showed that the dominant emission in both temperature regimes arose from stages where the 4f subshell was either almost or completely stripped. We also investigated if the effect of low density favours transitions to the lowest level as observed in recently reported results.

Annealing effect on the chemical structure of diamondlike carbon

The effect of annealing in an ultrahigh vacuum on the chemical structure of diamondlike carbon (DLC) was investigated using photoelectron spectroscopy, thermal desorption spectroscopy, electrical resistivity, and micro-Raman spectroscopy measurements. The line shapes of the C 1s photoelectron spectra depended on annealing temperature. The relative intensities of four chemical components in the spectra were quantitatively evaluated: sp3 carbon with carbon-carbon bonds (C–C sp3 carbon), sp2 carbon with carbon-carbon bonds (C–C sp2 carbon), sp2 carbon with hydrogen-carbon bonds (H–C sp2 carbon), and sp3 carbon with hydrogen-carbon bonds (H–C sp3 carbon). The variation of the ratio of the components demonstrated that hydrogen in DLC is emitted to the outside in between 450 and 600 °C, and the remaining DLC is graphized above 600 °C. The increase in the asymmetry of the C 1s spectra and the decrease in the electrical resistivity of the DLC film with annealing temperature agree with the picture that the H–C bon...

Fabrication of nanohole array on Si using self-organized porous alumina mask

Formation of the ordered array of nanoholes on Si was investigated by the use of the self-organized porous alumina nanoholes array etching mask that is directly formed on the Si substrate by sputtering and subsequent anodic oxidation. Reactive ion etching using chlorine plasma against a porous alumina/thin-SiO2(10 nm)/Si substrate with a high self-bias of rf plasma was revealed to be very effective for pattern transfer to Si. After pattern transference a significant reduction of hole size was observed. In fact, the initial porous alumina hole size of 45 nm is reduced to 13 nm Si holes when the higher aspect ratio of porous alumina nanoholes mask is used. The etching characteristics strongly suggest that not only chemical etching but sputtering occurred, and that redeposition of nonvolatile materials in nanoholes plays an essential role in the reduction of the hole size.

Atomic Layer Controlled Digital Etching of Silicon

Layer-by-layer etching of silicon on atomic scale has been achieved by repeating the reaction cycles of fluorine (F) atom adsorption on a cooled Si surface and subsequent Ar+ ion (20 eV) irradiation which induces fluorine/Si surface reactions. The digital etch rate first increases and reaches a plateau region with an increase of Ar+ ion irradiation time. For the case of CF4/O2 downstream plasma as a fluorine source, CFx radical accumulation appears to be a self-limiting stop of the F/Si reaction to promote atomic layer etching, while F atoms produced by a remote NF3 plasma or an F2/95%He discharge also cause similar atomic layer etching in which the amount of physiosorbed fluorine molecules on Si surfaces controls the etch rate. The etching in the plateau region exhibits no microloading effect because the fluorine coverage is independent of pattern size. Anisotropic etching of Si with a 20 nm PMMA mask pattern and an aspect ratio of 5 is attained.