Dissolution behaviour of the barrier layer of porous oxide films on aluminum formed in phosphoric acid studied by a re-anodizing technique

Chemical dissolution of the barrier layer of porous oxide films formed on aluminum foil (99.5% purity) in the 4% phosphoric acid after immersion in 2 mol dm⁻³ sulphuric acid at 50 °C has been studied. The barrier layer thickness before and after dissolution was determined using a re-anodizing technique. A digital voltmeter with a computer system was used to record the change in the anode potential with re-anodizing time. It has been found that the barrier layer material may consist of two or three regions according to the dissolution rate. The barrier oxide contains two layers at 35 V: the outer layer with the highest dissolution rate and the inner layer with low dissolution rate. The barrier oxide contains three layers at 40 V and above it: the outer layer with high dissolution rate, the middle layer with the highest dissolution rate and the inner layer with low dissolution rate. It has been shown that there is a dependence of the dissolution rate on the surface charge of anodic oxide film. Annealing of porous alumina films for 1 h at 200 °C leads to disappearance of layers with different dissolution rates in the barrier oxide. We explained this phenomenon by the absence of the space charge in the barrier oxide of such films.     

Electrochemical oxidation of La2CuO4 thin films grown by molecular beam epitaxy

Thin insulating and c-axis oriented films of La₂CuO₄ are grown using a molecular beam epitaxy technique. Subsequently, these films are oxidized electrochemically using a 1N KOH solution. This approach is used to induce superconductivity, leading to a maximum T_c0 of 31 K,, measured both resistively and inductively. The surface morphology, lattice constants and the resistivity before and after the electrochemical treatment are compared.     

Development of porous metal oxide thin films by co-evaporation

This paper focuses on the development of mixed metal oxide thin films and physical characterization of the films. The films were produced by co-evaporation of titanium oxide and tungsten oxide powders. This allowed the development of titanium oxide-tungsten oxide films as analyzed using XPS. Examination in the SEM and AFM showed that the films were nanoporous with the pore size and pore orientation varying as a function of the deposition angle. UV-vis spectra of the films show an increase of transmittance with increasing deposition angle which is attributed to the structure and porosity of the films. Raman analysis indicated that the as-deposited films have broad and weak Raman characteristics, attributed to the nanocrystal nature of the films and the presence of defects, and the peak broadening deceases after annealing the film, as expected.     

Aluminium oxide thin films prepared by plasma-enhanced chemical vapour deposition

Thin films of aluminium oxide have been deposited on glass, quartz, Si(100), steel, nickel, and aluminium by plasma-enhanced chemical vapour deposition (PECVD) using aluminium acetylacetonate (Al(acac)₃) as precursor. The deposits are hard (up to 2370 HK) and show good adherence to the substrates. The influence of various experimental parameters on deposition rate, film composition and hardness has been studied. The bias turned out to be the most effective parameter.On leave from Beijing Solar Energy Research Institute, Beijing, P.R. China     

Effect of surface roughness of chitosan-based microspheres on cell adhesion

Microspheres are novel candidate materials for microcarriers and tissue-engineering scaffolds. Chitosan microspheres were selected as the base materials because of their excellent properties for biomedical applications. But their smooth surfaces were not adapted for cell attachment. Hence, in order to improve the roughness of chitosan microspheres, β-TCP/chitosan composite microspheres were developed. From SEM photographs, the coarse surfaces of composite microspheres were observed, there were some ceramic particles standing out of the chitosan matrix. And their roughness measured by profilometers was about 2.0 μm. Mouse MC3T3-E1 osteoblasts were seeded on the microspheres for evaluating the attachment interaction between cells and materials. According to the ESEM photographs and MTT assay, the adherence and proliferation of osteoblasts on the surfaces of modified microspheres were better than those on the chitosan microspheres, which were mainly attributed to the improved roughness of surface.     

Electrochemical synthesis of polypyrrole/carbon nanotube nanoscale composites using well-aligned carbon nanotube arrays

Polypyrrole/carbon nanotube nanoscale composites were successfully fabricated by electrochemical deposition of polypyrrole over each of the carbon nanotubes in well-aligned large arrays. The thickness of the polypyrrole coating can be easily controlled by the value of the film-formation charge. For both thin (low film-formation charge) and thick (high film-formation charge) films, the polypyrrole coating on the surface of each nanotube is very uniform throughout the entire length, as observed by transmission electron microscopy. Received: 2 May 2001 / Accepted: 4 May 2001 / Published online: 20 June 2001     

Field emission behavior of cuboid zinc oxide nanorods on zinc-filled porous silicon

Single-crystalline zinc oxide (ZnO) nanorods with cuboid morphology have been prepared on the zinc-filled porous silicon substrate using a vapor phase transport method. Field-emission measurements showed that the turn-on field and threshold field of the cuboid ZnO nanorods film were about 3.2 and 8.2 V/μm respectively. From the emitter surface, a homogeneous emission image was observed with emission site density (ESD) of ∼10⁴ cm⁻². The better emission uniformity and the high ESD may be attributed to a large number of ZnO nanocrystallites as emitter on the surface of the nanorod end contributing to emission.     

Thin films of magnesium oxide prepared by plasma-enhanced chemical vapour deposition

Thin films of magnesium oxide have been deposited on glass, quartz, stainless steel, and nickel by plasma enhanced chemical vapour deposition using 2,2,6,6-tetramethyl-heptanedionato-3,5-magnesium(II) (Mg(thd)₂) as precursor. The films show (100)-orientation when deposited at temperatures 673 K. The influence of experimental parameters on deposition rate and film properties has been studied.On leave from the Beijing Solar Energy Research Institute, Beijing, China     

Demineralisation of semi-anthracite char with molten salts/HCl: Effects on the porous texture and reactivity in air

The effects of chemical heat treatments of a semi-anthracite char (AC) on textural properties and reactivity in air of the material are investigated. The starting char was first treated with a mixture of LiCl/KCl or LiCl/KCl/CaO at 743, 873 or 1173 K and the products obtained were then washed thoroughly with distilled water. A small fraction of these samples were treated with 10⁻³ M HCl solution. Valuable information on textural modifications produced in the material was derived from the adsorption isotherms for CO₂ at 273 K. The reactivity tests were carried out at 808, 823 and 823 K. The microporosity developed and the reactivity in air increased in the partially demineralised products. The former effect was stronger for the LiCl/KCl/CaO-treated samples and the latter for a larger number of the LiCl/KCl-treated samples.     

Synthesis of Y-junction carbon nanotubes within porous anodic aluminum oxide template

Y-junction carbon nanotubes with the average diameter about 200 nm were successfully synthesized within porous anodic aluminum oxide template, which was prepared by anodic anodizing aluminum sheet in 1.0 mol/l H₃PO₄ solution at a constant anodization voltage 90 V.     

Scribing and cutting a blue LED wafer using a Q-switched. Nd:YAG laser

Chemical doping of single-wall carbon nanohorns (SWNHs) with K and Br was examined by vapor-phase reaction and studied by Raman scattering. Electro-chemical Li-ion doping using an electrolyte of LiAsF₆ in a mixture (1:1 by volume) of ethylene carbonate and diethyl carbonate was also carried out. All these experiments indicate that an anomalously small charge transfer occurs in saturation-doped SWNHs using these reagents, in sharp contrast to the behavior observed for single-wall carbon nanotube bundles and graphite. This rather remarkable result is not understood at present. Received: 13 July 2000 / Accepted: 14 July 2000 / Published online: 5 October 2000     

Catalysis of dispersed silver particles on directional etching of silicon

Silver particles are dispersed on silicon by magnetron sputtering and post-annealing to investigate the catalytic effects of individual silver particles on wet etching of silicon surface. According to scanning electron microscopy, dispersed deep holes are present and the major etching direction is vertical to the surface of a Si(1 0 0) wafer or inclined to that on a Si(1 1 1) wafer. Our experiments indicate that the effect of the anisotropy of Si on directional etching is fundamental and the wafer resistivity and experimental process have important influence on the etching results. In addition, aggregation of silver particles and random horizontal etching on the surface of the wafer are caused by the local imbalance between the oxidant and HF. Our results enable better understanding of the catalytic effects of metal particles on silicon and are helpful to the preparation new silicon nanostructures.     

Pulsed laser deposition of polyhydroxybutyrate biodegradable polymer thin films using ArF excimer laser

We demonstrated the pulsed laser deposition (PLD) of high quality films of a biodegradable polymer, the polyhydroxybutyrate (PHB). Thin films of PHB were deposited on KBr substrates and fused silica plates using an ArF (λ = 193 nm, FWHM = 30 ns) excimer laser with fluences between 0.05 and 1.5 J cm⁻². FTIR spectroscopic measurements proved that at the appropriate fluence (0.05, 0.09 and 0.12 J cm⁻²), the films exhibited similar functional groups with no significant laser-produced modifications present. Optical microscopic images showed that the layers were contiguous with embedded micrometer-sized grains. Ellipsometric results determined the wavelength dependence (λ ∼ 245-1000 nm) of the refractive index and absorption coefficient which were new information about the material and were not published in the scientific literature. We believe that our deposited PHB thin films would have more possible applications. For example to our supposal the thin layers would be applicable in laser induced forward transfer (LIFT) of biological materials using them as absorbing thin films.     

Effect of the current density on the volume expansion of the deposited thin films of aluminum during porous oxide formation

The effect of the anodic current density, temperature and concentration of the oxalic acid on the volume expansion of porous alumina films formed from 1.8 μm thick aluminum films has been investigated. The volume expansion of the aluminum during oxidation was determined by the step height between the aluminum surface and the porous alumina surface at the edge of the anodized region, which was measured with a mechanical profiler with computer signal processing. Experiments showed, that the volume expansion factor as well as the cell dimensions is proportional to the anodizing voltage. The dependence of the volume expansion factor (k) on the anodizing voltage (U) has the linear nature. The volume expansion factor in the 4% solution of oxalic acid can be defined by the following equation: k=1.092+0.007U. It was established, that the dependence of the logarithm of the ion current density on the inverse volume expansion factor of porous alumina has the linear nature.     

Platelet adhesion on phosphorus-incorporated tetrahedral amorphous carbon films

The haemocompatibility of phosphorus-incorporated tetrahedral amorphous carbon (ta-C:P) films, synthesized by filtered cathodic vacuum arc technique with PH₃ as the dopant source, was assessed by in vitro platelet adhesion tests. Results based on scanning electron microscopy and contact angle measurements reveal that phosphorus incorporation improves the wettability and blood compatibility of ta-C film. Our studies may provide a novel approach for the design and synthesis of doped ta-C films to repel platelet adhesion and reduce thrombosis risk.     

Oxidizing agent concentration effect on metal-assisted electroless etching mechanism in HF-oxidizing agent-H2O solutions

The mechanism of metal-assisted electroless etching of silicon in HF-oxidizing agent-H₂O etching system as a function of oxidizing agent concentration was studied. Three types of oxidizing agent were experimented namely Na₂S₂O₈, K₂Cr₂O₇ and KMnO₄. Their concentrations were varied from 0.05 M to 0.3 M. The layers formed on silicon were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD) and energy-dispersive X-ray (EDX). It is shown that an insoluble solid-phase film (K₂SiF₆) form on silicon surface when concentration of K₂Cr₂O₇ or KMnO₄ increases in chemical solutions. On other hand, when Na₂S₂O₈ concentration increases, the surface roughness decreases without any chemical complex formation.     

Investigation on bio-mineralization of melt and sol-gel derived bioactive glasses

The bio-mineralization properties of the melt-derived bioactive glass 45S5 and the sol-gel derived bioactive glasses 58S and 77S were investigated and compared using in vitro test combined with BET, XRD, FTIR and SEM techniques. It was found that the surfaces of the three bioactive glasses could be mineralized by immersion in a simulated body fluid (SBF) at 37 °C for several hours. The bio-mineralized products on the surfaces of the bioactive glasses were apatite microcrystals with a low crystallinity, but the composition and morphologies of the apatite microcrystals on three glasses were different.     

Water electrolysis-induced optical degradation of aluminum-doped zinc oxide films

A type of optical degradation of aluminium-doped zinc oxide (AZO) films due to water electrolysis-induced reduction reaction was reported. An experiment was designed in which AZO films were immersed in a 0.01 M NaOH aqueous solution as cathode to electrolyze water. Significant decreases in the optical transmission of the treated samples were observed. Studies by X-ray diffraction and scanning electron microscope showed that the degradation of AZO films was due to compositional and structural changes with the treatment of water electrolysis, which resulted from the reduction reaction of atomic hydrogen generated in the electrolysis of water. This optical degradation reflects the stability degradation of AZO films under water electrolysis environment.     

The effect of chemical treatment on apatite-forming ability of the macroporous zirconia films formed by micro-arc oxidation

Macroporous and nano-crystalline zirconia film was prepared by micro-arc oxidation (MAO) of zirconium, and the effect of chemical treatment in H₂SO₄ or NaOH aqueous solutions on the microstructure and apatite-forming ability of the film was investigated. Compared with the MAO film, the chemically treated films do not exhibit apparent changes in phase component, morphology and grain size, however, have more abundant basic Zr-OH groups. The films treated with H₂SO₄ and NaOH solutions can induce apatite formation on their surfaces in simulated body fluids (SBF) within 1 day, whereas no apatite was detected on the untreated ZrO₂ surface by 30 days. It is believed that the enhanced apatite-forming ability of the chemically treated ZrO₂ films is related to the abundant basic Zr-OH groups on their surface.     

Pattern Formation in a Vibrated Granular Layer on an Inclined Base

We carry out the simulations of pattern formation in a two-dimensional vibrated granular layer on an inclined base by molecular dynamics. It is found that the maximum amplitude of the pattern is greater at the lower part than at the higher part of the base, and is proportional to the thickness of the layer. Meanwhile, the wavelength varies non-monotoniclly as the inclined angle of the base is increased.