Phase Composition of Films Deposited by ZrB2 RF Magnetron Sputtering

X-ray diffraction and electron-microscopic studies demonstrate that the conditions of ZrB₂ rf magnetron sputtering (primarily, the argon pressure) have a significant effect on the thickness, phase composition, and structure of the growing films. The films deposited on silicon substrates at low argon pressures (0.15–0.18 Pa) consist of zirconium diboride and a very thin zirconia layer. At higher argon pressures, from 0.21 to 0.42 Pa, the film thickness is larger, and the film is composed of four layers: ZrB₂/ZrB/ZrO₂/B₂O₃. Increasing the argon pressure to 0.47 Pa, reduces the deposition rate and the thickness of the zirconia layer. The resultant films contain neither ZrB nor B₂O₃. At still higher argon pressures, up to 0.65 Pa, film thickness continues to decrease because of the reduction in the thickness of the ZrB₂ layer. The substrate temperature influences the structural perfection of the growing films. Other sputtering parameters influence the argon pressure and, accordingly, the phase composition of the films. At deposition temperatures of 60–70°C, there are certain orientational relationships between the films and single-crystal substrates. On glass-ceramic substrates, the deposition rate is substantially faster, and the deposits consist of randomly oriented crystallites.     

Preparation and Characterization of Epitaxial-Grown Ba0.65Sr0.35TiO3 Thin Films by the Sol-Gel Process on Pt/MgO Substrates

Epitaxial-grown barium-strontium-titanate (BST, Ba_0.65Sr_0.35TiO₃) thin films have been successfully deposited on Pt/MgO (100) substrates using sol-gel techniques. Crack-free 350-nm-thick films were fabricated using a multilayer spinning technique and calcination at 650°C in oxygen for 1 hr. The X-ray diffraction pattern showed that (001) planes of BST films were mainly laid parallel to Pt (100) and MgO (100). The dielectric constant and dissipation factor for BST thin films at a frequency of 10 kHz were 480 and 0.02, respectively. The results of the temperature-dependence of the dielectric constant and dissipation factor showed that sol-gel–derived BST films had Curie temperatures of about 35°C and diffused ferroelectric phase transition characteristics. The leakage current density through the BST films was about 2.75 × 10^–7 A/cm² at an applied voltage of 3 V. The BST films exhibited a well-saturated ferroelectric hysteresis loop with remnant polarization P _r = 2.8 C/cm² and coercive field E _c = 52 kV/cm.     

The effect of test temperature on the intergranular cracking of Nb-A286 alloy in low cycle fatigue

The continuous low cycle fatigue behaviors of a Fe-base superalloy, Nb-modified A286 alloy, have been evaluated at the test temperatures of 650°C and 350°C under various total strain ranges. It was found that the change of the slope in the Coffin–Manson plot was closely related to the fatigue cracking with the test temperature. In the high temperature low cycle fatigue (HTLCF) of Nb-A286 alloy, the fatigue cracking exhibited the intergranular mode at 650°C and the transgranular mode at 350°C. The intergranular fatigue cracking at 650°C was due to the precipitation of the phase at the grain boundary assisted by the applied stress during low cycle fatigue. It is investigated whether the precipitate at the grain boundary provides the site for the grain boundary cavitation, which induces the intergranular cracking in low cycle fatigue. This is confirmed by the results of low cycle fatigue at 25°C after heat treatment which forms the phase at the grain boundary.     

Temperature effects on the properties of Ge thin films

The effects of substrate temperature (T_s) on the properties of vacuum evaporated p-type Ge thin films have been investigated for 25s<400°C. Increase in the substrate temperature improves the crystallinity and increases the grain size resulting a gradual change from amorphous to polycrystalline structure which was attained above a substrate temperature of 225°C. Low resistive (1×10^–2 ohm-cm) and high mobility (280 cm²/V·s) films were obtained at T_s=400°C. It has been observed that the conduction mechanism in polycrystalline films was dominated successively by hopping, tunneling and thermionic emission as the sample temperature was increased from 40 to 400 K. In amorphous samples, conduction was described in terms of different hopping mechanisms.     

Electrical Activity of Native Defects in n-Type ZnSe Crystals

The transport properties of n-type ZnSe crystals annealed in liquid Zn at temperatures from 600 to 950°C are studied in the range 55–500 K. As the annealing temperature increases to above 650°C, the concentration of shallow donors rises sharply, their ionization energy decreases from 28 to 9 meV, and the compensation ratio drops from 0.91 to 0.35. The electrical conductivity of the crystals annealed at low temperatures is determined by shallow donors such as Al_Zn, Ga_Zn, and In_Zn. At annealing temperatures above 800°C, the concentration of zinc vacancies, compensating the shallow donors, decreases sharply, whereas the concentration of selenium vacancies, which act as shallow donors and determine the electrical conductivity of the crystals, rises markedly. Reducing the annealing temperature to below 650°C drastically decreases the conductivity and electron concentration of the samples and leads to anomalously low carrier mobilities. The observed anomalies in the transport properties of illuminated n-type ZnSe crystals are interpreted in terms of a random impurity potential.     

Electrical properties of non c-axis oriented SrBi2(Ta0.95V0.05)2O9 thin films

Pulsed laser deposition technique was used to grow off c-axis oriented SrBi₂(Ta_0.95V_0.05)₂O₉ (SBTV) ferroelectric thin films. X-ray diffraction studies revealed the c-axis suppression in the films grown at lower substrate temperature (350°C) followed by annealing at higher temperatures (650°C). In-plane lattice parameters of the films were decreased with increase in annealing temperature. SBTV films annealed at 750°C exhibited enhanced ferroelectric properties with remanent polarization (2P _r) of 31.5 C/cm² and coercive field (E _c) of 157 kV/cm. The dielectric permmitivity of the films increased with increase in annealing temperature and it was attributed to the grain size dependence. The films annealed at 750°C showed maximum value of dielectric permittivity 172 with a tangential loss of 0.1, at 100 kHz. Higher value of dissipation factor at lower annealing temperature is explained in terms of space charge accumulation at grain boundaries. The leakage current densities of the films follow ohmic behavior at low field regime and space charge limited current dominates at higher fields.     

Preparation of Thick LaCu1 – x Ni x O2.5 + δ Films Exhibiting a High-Temperature Metal–Semiconductor Transition

The conditions for producing thick LaCu_{1 – x} Ni _x O_{2.5 +} films on different substrates were optimized. The effects of the heat-treatment conditions, substrate material, and the nature of the liquid organic binder on the composition, structure, and properties of the films were studied. Single-phase coatings obtained on MgO, ZrO₂, BaSO₄, and Ni substrates 50 to 200 m in thickness were close in properties to bulk LaCu_{1 – x} Ni _x O_{2.5 +} and exhibited a metal–semiconductor transition at about 500°C.     

Characterization of hydroxyapatite powders prepared by ultrasonic spray-pyrolysis technique

The hydroxyapatite (HAp) powder was prepared by the ultrasonic spray-pyrolysis technique; the characterization of the resulting powders was performed. Five kinds of the starting solutions with the Ca/P ratio of 1.67 were prepared by mixing Ca(NO₃)₂, (NH₄)₂HPO₄ and HNO₃; the concentrations of Ca²⁺ and PO₄ ^3– were in the ranges of 0.10 to 0.90 mol·dm^–3 and 0.06 to 0.54 mol·dm^–3, respectively. These solutions were sprayed into the heating zone to prepare the HAp powders. The heating zone was composed of two electric furnaces; the lower furnace was used for the evaporation of the solvent from the droplets (300–500°C) and the upper furnace for the pyrolysis of the precipitated metal salts (750–900°C). The easily sinterable HAp powder was prepared by spray-pyrolysing the solution with Ca²⁺ (0.50 mol·dm^–3) and PO₄ ^3– (0.30 mol·dm^–3) at the temperatures of 800°C (the upper furnaces) and 400°C (the lower furnaces). The resulting powder was composed of the spherical particles with diameters of 1 m or below. Even without the calcination and grinding operations, the relative densities of the compacts fired at 1150 and 1200°C for 5 h attained maxima 95%. The microstructure of the sintered compacts appeared to be uniform; the average grain size was 3 m. The activation energies for the grain growth of the sintered HAp compacts were 120 to 147 kJ · mol^–1 · K^–1.     

Structural and electrical properties of cadmium-sulpho-selenide solid solutions

Complete solid solutions of CdS _x Se_1–x (0x1) were synthesized by vacuum fusion of stoichiometric proportions of CdS and CdSe. X-ray diffraction data revealed that they possess the hexagonal wurtzite structure. The unit cell lattice constants vary linearly with the composition parameter,x, following Vegard's law.Thin films of CdS _x Se_1–x (0x1) solid solutions could be deposited onto glass substrates by thermal evaporation of the bulk material in 10^–4 Pa vacuum. Structural investigation showed that the films are polycrystalline with predominant appearance of the (002) reflecting plane. On annealing at 250°C in 10^–2 Pa vacuum atmosphere, aggregation and rearrangement of the as-deposited tiny crystallite occurred, preserving the same crystal structure.The dark electrical resistivity of the films is independent on the film thickness, but it varies appreciably with the composition parameter,x, showing a minimum resistivity of 0.02 cm atx=0.55. The temperature dependence of the resistivity follows the semiconducting behaviour with an extrinsic and an intrinsic conduction below and above 70°C, respectively. The determined activation energies 0.2 eV and 0.8 eV, respectively, correspond to shallow and deep trap levels, respectively.     

Thermodynamic Modeling of BC x N y Chemical Vapor Deposition in the B–C–N–H System

Thermodynamic analysis of the chemical vapor deposition of BN-based films in the B–C–N–H system was carried out for reduced pressures (133 and 1.33 Pa) and a wide temperature range (300–1300 K). The results indicate that, using mixtures of trimethylamineborane, (CH₃)₃N · BH₃, with H₂, NH₃, or N₂, one can produce films of various compositions: from BN to mixtures of BN, carbon, and boron carbide.     

Phase Relations in the Bi–(Pb)–Sr–Ca–Cu–Sc–O System

The phase relations in the Bi–(Pb)–Sr–Ca–Cu–Sc–O system were studied near Bi₂Sr₂CaCu₂O_{8 +} (Bi-2212) and (Bi,Pb)₂Sr₂Ca₂Cu₃O_{10 +} (Bi-2223) between 850 and 930°C. The introduction of Sc led to the formation of a new compound Sr₂ScBiO₆, which coexisted with Bi-2212 and Bi-2223. Using crystallization from a peritectic melt at different cooling rates, we obtained Bi-2212 matrix composites containing finely dispersed Sr_1.9Ca_0.1ScBiO₆inclusions, with T _cattaining 89 K. The T _cof the Bi-2223–Sr_1.9Ca_0.1ScBiO₆superconducting ceramic prepared by solid-state sintering of a Bi–(Pb)–Sr–Ca–Cu–Sc–O precursor was 108.5 K.     

Ferroelectric Lead Zirconate Titanate Films Prepared by Spray Pyrolysis of Carboxylate Solutions

Ferroelectric PbTi_0.6Zr_0.4O₃films 0.5–1.5 m in thickness were produced on platinum substrates by spray pyrolysis of carboxylate solutions. The optimized compositions of the precursor solutions, containing methacrylic acid and ethylene glycol, are stable under normal conditions, allow the annealing temperature to be reduced, and lead to higher quality film surfaces and large grains. The film exhibit the following electrical properties: T _C= 360–460°C, _max= 1750 at T _C, tan = 0.02–0.1 at 1 kHz and room temperature, P _{s max} = 18 C/cm², P _{r max} = 15 C/cm²at 50 Hz, and E _c= 42–120 kV/cm.     

Synthesis, crystal structure and X-ray powder diffraction data of the phosphor matrix 4SrO·7Al2O3

The white phosphor matrix 4SrO·7Al₂O₃ has been synthesized by firing the appropriate mixture of SrCO₃, Al(OH)₃ and H₃BO₃ in the molar ratios 1:3.5:0.135 at 1300°C for 4–7 h. The crystal structure of 4SrO·7Al₂O₃ has been determined as a orthorhombic Pmma space group with a=24.7451(2)Å, b=8.4735(6)Å, c=4.8808(1)Å, V=1023.41(3)ų, Z=2, and D=3.66 g cm^–3 by the Rietveld analysis. The refinement figures of merit are R_p=8.26, R_wp=11.60, R_bragg=4.44 and s=2.61 for 844 reflections with 2<119.94°. And the corresponding X-ray powder diffraction data are presented for search/match analysis.     

Preparation of Si3N4 whiskers by reaction of wheat husks with NH3

-Si₃N₄ whiskers that are 1–10 mm long and 0.5–1.1 m thick were obtained by the reaction of wheat husks with NH₃ at 1250–1450 °C. A maximum whisker yield of about 30% was obtained at 1450 °C with the addition of an iron impurity. Whiskers with 1.3–2.2 m thickness (average 1.6 m) were obtained by the addition of an H₂S impurity. Thin whiskers with periodic thick and thin diameters were also obtained.     

Corrosion of Iron in a Carbonate-Bicarbonate Solution. Part 1. Crystallographic Analysis of Passive Films

Visible passive films are formed on the surface of 1010 steel at 325K in a solution of 1N NaHCO₃ + 1N Na₂CO₃ at anodic potentials up to –320mV_NHE inclusively. For potentials below –400mV, they are dull and contain FeCO₃. For –(390–320)mV, the films are thin blackish bright. Most probably, the diffraction peaks are caused by Fe₃O₄–Fe₂O₃. For –(430–400)mV, the films are dull blackish. Probably, this color is caused by a composite of magnetite and siderite.     

Discrete β-Ta2O5 crystallite formation in reactively sputtered amorphous thin films

The crystallization of thin amorphous TaOx films formed by d.c. reactive sputtering was investigated at temperatures from 500–700 °C. The films remained amorphous for times up to 100 h at 500 °C. The formation of discrete, single crystallites of the orthorhombic -Ta2O5 phase was observed after annealing at 600 °C for times from 8–108 h. The crystallites were 0.35 m×0.35 m after 8 h and grew to approximately 2.5 m×2.0 m after 108 h. A (2 0 0) fibre texture with a 6° spread was observed. More rapid in-plane growth in the [0 1 0] direction resulted in a near-rectangular shape and is attributed to a ledge growth mechanism. Higher temperature anneals at 650 and 700 °C produced less-textured polycrystalline films with remnant amorphous regions. © 1998 Kluwer Academic Publishers     

Phase Relations in the Cu–Sb–O System

The Cu–Sb–O system was studied by x-ray diffraction and thermal analysis between 700 and 1000°C. The compositions of copper antimonates were refined. Sb₂O₄ was found to exist in two polymorphs above 800°C: -Sb₂O₄ (dominant phase) and -Sb₂O₄. The evolution of phase equilibria with increasing temperature was examined. The isothermal sections of the Cu–Sb–O phase diagram were mapped out using new and earlier reported results.     

Effect of pH on 980 °C spinel phase-mullite formation of Al2O3-SiO2 gels

Different reaction paths of mullite formation via sol-gel processing techniques are reviewed. These variations are due to differences in hydrolysis/gelation behaviours of the silica and alumina components used. Variations of pH during processing without altering other variables follow three different routes of mullite formation. In the highly acidic region(pH 1), the gel does not exhibit a 980 °C exotherm but forms -Al₂O₃. Mullite forms at high temperature by diminution of -Al₂O₃ and -cristobalite, respectively. In the pH range of 3–4.5, gels exhibit a 980 °C exotherm and develop only mullite. In the highly alkaline region (pH 14), the gel produces a Si-Al spinel phase at the 980 °C exotherm and mullite formation at the 1330 °C exotherm takes place from the intermediate Si-Al spinel phase.     

Preparation and electrical properties of ITO thin films by dip-coating process

Indium tin oxide (ITO) thin films were prepared on quartz glass substrates by a dip-coating process. The starting solution was prepared by mixing indium chloride dissolved in acetylacetone and tin chloride dissolved in ethanol. The ITO thin films containing 0 20 mol% SnO₂ were successfully prepared by heat-treatment at above 400 °C. Chemical stability of sol were investigated by using a FTIR spectrometer. The electrical resistivity of the thin films decreased with increasing heat-treatment temperature, that is carrier concentration increased, and mobility decreased with increasing SnO₂ content. The ITO thin films containing 12 mol% SnO₂ showed the minimum resistivity of =1.2 × 10^–3 ( cm). It also showed high carrier concentration of N=1.2 × 10²⁰(cm^–3) and mobility _H=7.0(cm² V^–1 s^–1).     

Optical constants and electrical conductivity of Ge20Se60Sb20 thin films

Optical absorption and electrical resistivity of amorphous Ge₂₀Se₆₀Sb₂₀ films are investigated as a function of the thermal annealing. The dependence of the optical absorption coefficient on the photon energy is ascribed by the relation (h) = B(h–E_o)². Increasing the annealing temperature from 423 K to 553 K, decreases the optical gap of the film from 1.25 eV to 0.78 eV. The effect of annealing temperature on high frequency dielectric constant () and carrier concentration (N) was also studied. As a result of annealing the film at 533 K, the electrical resistivity and activation energy for conduction decreased from 5.7 × 10⁷ to 2.9 × 10² ·cm and from 0.94 to 0.34 eV, respectively. The crystalline structures resulting from heat treatment at different elevated temperatures have been studied by X-ray Diffraction (XRD). The optical and electrical changes were attributed to the amorphous-crystalline transformations in the chalcogenide films.