Physico-chemical and electrochemical characterization of Ti/RhOx–IrO2 electrodes using sol–gel technology

Sol–gel technology has been successfully used for the incorporation of RhO_x–IrO₂ on a Ti substrate. RhO_x–IrO₂ was prepared from chloride precursors of Rh and Ir, for surface studies. These metal oxides were then immobilised on solid Ti substrates via dip withdrawal coating methods to form thin films. The Ti/RhO_x–IrO₂ thin films were extensively characterized in terms of surface characterization and chemical composition and used in the oxidation of phenol. Thermo-gravimetric analysis (TGA) determined the calcination temperature at 700 °C where no further structural changes occurred due to mass loss. The rhodium oxide showed two-phase formations, RhO₂ and Rh₂O₃, which were attributed to high calcinated temperatures compare to one phase IrO₂ which was stable at lower temperatures. The scanning electron microscopy (SEM) showed that the morphology of the film was found to be rough with a grain-like appearance in the 150-nm range. The phase composition of these metal oxides was determined by X-ray diffraction (XRD) technique and found to have crystalline structures. The results obtained from Rutherford backscattering spectrometry (RBS) revealed information regarding the chemical composition of the metal oxides and confirmed the diffusion of Rh and Ir into the Ti substrate. Electrochemical characterization of the Ti/RhO_x–IrO₂ electrode, via cyclic voltammetry (CV), showed distinctive redox peaks: anodic and cathodic peaks associated with the oxidation and reduction of the ferricyanide–ferrocyanide couple was seen at 250 and 100 mV respectively; the peak observed at 1000 mV was associated with oxygen evolution and a broad reductive wave at −600 mV can be ascribed to the Ti/RuO_x–IrO₂ reduction, which proved that the Ti/RhO_x–IrO₂ electrode were electroactive and exhibit fast electrochemistry.     

Hydrogen-acetylene gas ratio and catalyst thickness effect on the growth of uniform layer of carbon nanotubes

Effect of catalyst thickness (2, 4, and 6 nm) and acetylene-hydrogen gas ratio (1/4, 2/4, and 3/4) on the synthesis of carbon nanotubes is reported in this article. Synthesized nanotubes are characterized by X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy, and Raman effect. From SEM results, nanotubes growth is less for higher thickness, as at higher thickness catalyst nanoparticles agglomerate which suppress the growth of nanotubes. Raman spectroscopy results reveal that at higher thickness defects density increases. Nanotube of better crystallinity and graphitic outer walls grows for lower acetylene-hydrogen gas ratio and at smaller thickness of catalyst layer. The sheet resistance of carbon nanotube thin film is measured by using Hall effect measurement systems. Smallest sheet resistance among synthesized multi-walled carbon nanotubes sample is obtained for nanotubes grown on 2 nm thick catalyst film and is 0.9 kΩ/square.     

GaAs/Si(100)异质外延4°偏角衬底对外延层结晶质量的提高

用低压金属有机物化学汽相沉积法(MOCVD)在Si(100)无偏角和Si(100)4°偏角衬底上外延生长GaAs层。异质外延采用两步生长法,并分别优化了两种衬底上的非晶低温缓冲层的生长条件。用X射线双晶衍射(XRD)和透射电子显微镜(TEM)对两种衬底上的GaAs外延层进行了结构表征,其中Si(100)4°偏角衬底上1.8μm厚GaAs的(004)面XRD衍射半高全宽338 arcsec,同比在无偏角衬底上的半高全宽为494arcsec,TEM图片显示4°偏角衬底上外延层中的位错密度大大降低。     

A hexane solution deposition of SnS2 films from tetrabutyltin via a solvothermal route at moderate temperature

SnS₂ films have been deposited on glass and alumina plate substrates by the reactions between an organotin precursor [tetrabuyltin, (CH₂CH₂CH₂CH₃)₄Sn] and carbon disulfide in n-hexane at the temperature range 180-200 °C for 10-40 h. The reaction system was oxygen free and applied at a moderate temperature. The films so prepared were characterized by techniques of X-ray diffraction, Scanning electron microscopy, Raman and Mössbauer spectroscopies. The films deposited on glass as well as on alumina plate have an average thickness of 30 μm, but have different rose-like morphologies, which are influenced by both the anisotropic growths of crystals and the different substrate structures. Photoluminescence measurements show that the films have an emission peak at approximately 590 nm.     

High-temperature stability of α-Ta4AlC3

Cold-pressed α-Ta4AlC3 powders were annealed up to 1750 °C to test first-principles predictions of α-β phase-stability reversal at 1600 °C. Up to 1600 °C, the α-Ta₄AlC₃ samples were stable with no indications of any α-β transformation, as shown by the strong characteristic X-ray diffraction peaks of α-Ta₄AlC₃ and the zigzag stacking observed by transmission electron microscopy. These results show that, in this experimental situation, high temperature alone is not sufficient to cause the α-β transformation.     

A coprecipitation technique to prepare ZnNb2O6 powders

A simple coprecipitation technique was successfully applied for the preparation of pure ultrafine single phase, ZnNb₂O₆ (ZN). Ammonium hydroxide was used to precipitate Zn²⁺ and Nb⁵⁺ cations as hydroxides simultaneously. This precursor on heating at 750°, produced ZN powders. For comparison, ZN powders were also prepared by the traditional solid state method. The phase contents and lattice parameters were studied by the powder X-ray diffraction (XRD). Particle size and morphology were studied by transmission electron spectroscopy (TEM).     

The effect of deposition parameters on the properties of yttria-stabilized zirconia thin films

Yttria-stabilized zirconia (YSZ) films were deposited by RF magnetron sputtering in order to examine the effects of sputtering conditions on the properties of the resulting thin-films. X-ray diffraction (XRD), Rutherford backscattering spectroscopy (RBS) and scanning electron microscopy (SEM) were used to characterize the films. Additionally, films were deposited on alumina bars to examine the effect of the coatings on the strength of a brittle substrate. RBS analysis indicated that the ratio of oxygen to zirconium in the films varied from 1.84 to 2.10. XRD showed that there was a wide variation in the amount of monoclinic and tetragonal phases that appeared to be related to the O:Zr ratio. Despite these variations, there was no significant difference found in flexural strength found among the groups of alumina bars that were coated with YSZ. The likely cause is the columnar grain morphology of the deposited thin-films, which does not allow strengthening mechanisms to become operative.     

Growth and optical and field emission properties of flower-like ZnO nanostructures with hexagonal crown

Flower-like zinc oxide (ZnO) nanostructures with hexagonal crown were synthesized on a Si substrate by direct thermal evaporation of zinc power at a low temperature of 600 °C and atmospheric pressure. Field emission scanning electron microscopy, transmission electron microscopy, X-ray diffraction, Raman spectroscopy and photoluminescence were applied to study the structural characteristics and optical properties of the product. The result indicated that the flower-like product with many slender branches and hexagonal crowns at the ends were single-crystalline wurtzite structures and were preferentially oriented in the <001> direction. The photoluminescence spectrum demonstrated a strong UV emission band at about 386 nm and a green emission band at 516 nm. The field emission of the product showed a turn-on field of 3.0 V/µm at a current density of 0.1 μA/cm², while the emission current density reached about 1 mA/cm² at an applied field of 5.9 V/μm.     

Structure–property correlation of pure and Sn-doped ZnO nanocrystalline materials prepared by co-precipitation

The structural, optical and electrical properties of pure and tin (Sn) doped zinc oxide (ZnO) nanocrystalline materials prepared by co-precipitation method have been studied as a function of Sn doping concentration. The phase identification through powder X-ray diffraction methods confirmed that pure and Sn-doped zinc oxide powder have typical hexagonal wurtzite structure (a = 3.407 Å and c = 4.592 Å) with slight change in lattice parameters. The surface morphological examination with field emission scanning electron microscopy revealed the fact that the grains are closely and densely packed and pores/voids between the grains decrease with increasing the doping concentration of Sn from 0% to 15%. The energy bandgap of pure ZnO was found to be 3.35 eV from optical absorption spectra obtained by ultraviolet–visible (UV–Vis) absorption spectrophotometer. The variation of energy bandgap and electrical resistivity of Sn-doped ZnO were also determined with tin doping. Upon increasing the Sn dopant concentration from 0 to 15 wt%, the optical bandgaps of ZnO increases from 3.35 to 3.42 eV. The electrical resistivity of Sn-doped ZnO has been decreased at least two orders of magnitude, i.e. from 1263.17 to 28.64 Ω cm. This decrement in electrical resistivity may be due to the partial substitution of divalent Zn²⁺ ions with tetravalent Sn⁴⁺ ions, generating more free electrons for conduction.     

Influences of Similar Elements on Glass Forming Ability and Magnetic Properties in Al-Ni-La Amorphous Alloy

Similar element substitution has been applied for improving glass forming ability (GFA) in Al₈₆Ni₉La₅ amorphous alloy. The effects of La-Ce and Ni-Co pairs on the GFA, magnetic properties and hardness of Al-Ni-La alloy were investigated by using X-ray diffraction (XRD), transmission electron microscopy (TEM), differential scanning calorimetry (DSC), magnetometer and hardness-tester. The results show the GFA of the samples in the order of Al86(Ni_0:5Co_0:5)9(La_0:5Ce_0:5)5< Al₈₆Ni₉La₅<Al₈₆Ni₉(La_0:5Ce_0:5)₅, implying that similar element substitution has a limited enhancing effect on the GFA of the present Al-Ni-La alloy. In addition, the measured samples display a diamagnetic behavior at room temperature. The variations of diamagnetic behavior as well as the microhardness of the samples are strongly dependent on the icrostructure, i.e., the amounts of the icosahedral structure and precipitates, after the similar element substitution in the Al-Ni-La alloy.     

Scanning transmission electron microscopy (STEM)-transmission electron microscopy (TEM) analysis of nitrogen ion implanted austenitic 302 stainless steel

The microstructure of nitrogen implanted AISI 302 austenitic stainless steel and the effect of long-term room temperature ageing on it have been studied. Samples were implanted in 1992 with 2.5×10²¹ N₂⁺ m⁻² at 130 keV. The characteristics of the implanted layer and the depth profile have been investigated by scanning transmission electron microscope combined with energy dispersive X-ray spectrometry. Electron diffraction patterns recorded in the implanted layer using transmission electron microscopy confirm the formation of CrN along with the presence of Cr₂N. The identification of phases by glancing angle X-ray diffraction also indicates the formation of Cr₂N and nitrogen solid solutions. The effects of ageing on the microstructure are observed to be small.     

Characterization of crystalline alumina films formed in alcohol-water solutions

Crystalline aluminum hydrous oxide [γ-AlO(OH)] thin films were prepared by hydration of a high cubicity tunnel-etched Al foil in alcohol—DI-water solutions at 95 °C for times up to 1 h. Presence of free molecular water was found to be an absolute requirement for film formation. In addition, the type of alcohol used in the hydration environment, n-propyl alcohol, ethylene glycol or glycerol, influenced the hydration kinetics, i.e. the induction time for film growth. Denser and low porosity films were suggested by field emission—scanning electron microscopy analysis. X-Ray diffraction showed the presence of only one crystalline phase identified as pseudoboehmite.     

Enhanced field emission characteristics of nitrogen-doped carbon nanotube films grown by microwave plasma enhanced chemical vapor deposition process

Nitrogen-doped carbon nanotube (CNT) films have been synthesized by simple microwave plasma enhanced chemical vapor deposition technique. The morphology and structures were investigated by scanning electron microscopy and high resolution transmission electron microscopy. Morphology of the films was found to be greatly affected by the nature of the substrates. Vertically aligned CNTs were observed on mirror polished Si substrates. On the other hand, randomly oriented flower like morphology of CNTs was found on mechanically polished ones. All the CNTs were found to have bamboo structure with very sharp tips. These films showed very good field emission characteristics with threshold field in the range of 2.65-3.55 V/μm. CNT film with flower like morphology showed lower threshold field as compared to vertically aligned structures. Open graphite edges on the side surface of the bamboo-shaped CNT are suggested to enhance the field emission characteristics which may act as additional emission sites.     

A low temperature route to prepare LaFeO3 and LaCoO3

A combination of digestion and further low temperature calcination to crystallize the product was employed to prepare LaFeO₃ (LF) and LaCoO₃ (LC) powders. Freshly co-precipitated lanthanum and ferric (or cobalt) hydroxide gels by sodium hydroxide were allowed to react at 100 °C under refluxing and stirring conditions for 4-6 h. These oven dried powders were heated at 450 °C to form crystalline LF (or LC) powders. The phase contents and lattice parameters were investigated by X-ray diffraction (XRD). Transmission electron microscope (TEM) investigations were carried out to examine the morphology and average particle size of these powders.     

Patterning crystalline indium tin oxide by high repetition rate femtosecond laser-induced crystallization

A method is proposed for patterning crystalline indium tin oxide (c-ITO) patterns on amorphous ITO (a-ITO) thin films by femtosecond laser irradiation at 80 MHz repetition rate followed by chemical etching. In the proposed approach, the a-ITO film is transformed into a c-ITO film over a predetermined area via the heat accumulation energy supplied by the high repetition rate laser beam, and the unirradiated a-ITO film is then removed using an acidic etchant solution. The fabricated c-ITO patterns are observed using scanning electron microscopy and cross-sectional transmission electron microscopy. The crystalline, optical, electrical properties were measured by X-ray diffraction, spectrophotometer, and four point probe station, respectively. The experimental results show that a high repetition rate reduces thermal shock and yields a corresponding improvement in the surface properties of the c-ITO patterns.     

A novel synthetic route to prepare cubic BN nanorods

Cubic boron nitride nanorods were prepared at 450°C by a low pressure benzene thermal synthesis method using BCl₃ and Li₃N as the reactants. The nanorods with various lengths and diameters were observed by transmission electron microscopy. The analysis of X-ray diffraction pattern and electron diffraction pattern revealed that the nanorods are cBN with a lattice constant of 3.62 Å. The Fourier transformation infrared spectra showed that the dominant phase is cBN, and the B:N ratio of 1.15:1 can be obtained from the X-ray photoelectron spectrum.     

Fatigue behavior of Zr-based bulk-metallic glasses

The objective of this paper was to study the fatigue characteristics of zirconium (Zr)-based bulk-metallic glasses (BMGs) and to investigate the mechanisms of fatigue-crack initiation, crack propagation, and fracture in BMGs. The fatigue ratios (fatigue limit/tensile strength) (0.30–0.55) of Zr-based BMGs were found to be generally comparable with those of crystalline alloys, such as steel and titanium alloys. Fatigue cracks typically initiate from shear bands, inclusions, and/or porosities. The striations resulting from the blunting and resharpening of the fatigue-crack tip formed in the fatigue-crack-growth region. The fine striation spacing seems to be comparable to that of the crystalline alloys.     

Impression creep behaviour of magnesium alloy-based hybrid composites in the transverse direction

The creep behaviour of a creep-resistant AE42 magnesium alloy reinforced with Saffil short fibres and SiC particulates in various combinations has been investigated in the transverse direction, i.e., the plane containing random fibre orientation was perpendicular to the loading direction, in the temperature range of 175–300 °C at the stress levels ranging from 60 to 140 MPa using impression creep test technique. Normal creep behaviour, i.e., strain rate decreasing with strain and then reaching a steady state, is observed at 175 °C at all the stresses employed, and up to 80 MPa stress at 240 °C. A reverse creep behaviour, i.e., strain rate increasing with strain, then reaching a steady state and then decreasing, is observed above 80 MPa stress at 240 °C and at all the stress levels at 300 °C. This pattern remains the same for all the composites employed. The reverse creep behaviour is found to be associated with fibre breakage. The apparent stress exponent is found to be very high for all the composites. However, after taking the threshold stress into account, the true stress exponent is found to range between 4 and 7, which suggests viscous glide and dislocation climb being the dominant creep mechanisms. The apparent activation energy Q_c was not calculated due to insufficient data at any stress level either for normal or reverse creep behaviour. The creep resistance of the hybrid composites is found to be comparable to that of the composite reinforced with 20% Saffil short fibres alone at all the temperatures and stress levels investigated. The creep rate of the composites in the transverse direction is found to be higher than the creep rate in the longitudinal direction reported in a previous paper.     

Photocatalytic degradation of selected dyes by titania thin films with various nanostructures

Titania thin films with various nanostructures of quasi-aligned nanorods, well-aligned nanotubes and nanoparticle aggregates were fabricated and utilized to assist photodegradation of three typical dye derivatives in water, i. e., rhodamine B (RB), methylene blue (MB) and methyl orange (MO). The thin films were characterized by X-ray diffraction, scanning electron microscope and UV-Vis diffuse reflectance spectra. It is found that the bandgap of most lab-fabricated thin films can be estimated more appropriately assuming a direct transition between the valance band and the conduction band of titania. The so-called natural ageing phenomenon was evidence for all the films to assist photodegradation of RB and MB in water; but not discernible for MO, which was much reluctant to photodegradation. MB decomposed much quickly than RB when assisted by titania with predominantly anatase; on the other hand, rutile favored the photodegradation of RB than that of MB. Titania thin films with top morphologies of quasi-aligned nanorods or nanotubes were found to possess advantageous turnover frequency and photonic efficiency over commercial P25 titania and sol-gel derived titania to assist photodegradation of RB and MB in water.     

Complex permeability and microwave absorbing properties of planar anisotropy carbonyl-iron/Ni0.5Zn0.5Fe2O4 composite in quasimicrowave band

Planar anisotropy carbonyl-iron (PACI)/Ni_0.5Zn_0.5Fe₂O₄ composite as absorbent filler in quasimicrowave band has been synthesized via ball-milling technique and solvothermal method. The effective permeability of the composite was measured and calculated. The result indicates that the magnetic loss in the composite is mainly caused by the natural resonance. Compared with the uncoated PACI particles, the permittivity of the composite decreased dramatically, and hence a dramatic enhancement of reflection loss (RL) was obtained in quasimicrowave band. This result indicates that our PACI/ferrite composite can be used as potential microwave absorbers in quasimicrowave band for its novel microwave properties.