Reaction of tantalum oxide with calcium chloride–calcium oxide melts

Tantalum oxide is a suitable precursor for electro-deoxidation, where a cathodic potential is applied to the oxide, immersed in a molten salt, to remove oxygen from the oxide leaving tantalum metal. The electro-deoxidation reactions take place in a melt of CaCl₂–CaO and, unlike the reduction of other metal oxides where little or no reaction occurs between the melt and oxide until the application of a cathodic potential, tantalum oxide readily reacts with the calcium oxide to form CaTa₄O₁₁, CaTa₂O₆ and Ca₂Ta₂O₇. These phases have completely different morphologies which convert a robust pellet into a collection of poorly connected particles.     

Effects of environment on creep behavior of two oxide/oxide ceramic–matrix composites at 1200 °C

The tensile creep behavior of two oxide/oxide ceramic–matrix composites (CMCs) was investigated at 1200 °C in laboratory air, in steam, and in argon. The composites consist of a porous oxide matrix reinforced with laminated, woven mullite/alumina (Nextel™720) fibers, have no interface between the fiber and matrix, and rely on the porous matrix for flaw tolerance. The matrix materials were alumina and aluminosilicate. The tensile stress–strain behavior was investigated and the tensile properties were measured at 1200 °C. Tensile creep behavior of both CMCs was examined for creep stresses in the 80–150 MPa range. Creep run-out defined as 100 h at creep stress was achieved in air and in argon for stress levels ≤100 MPa for both composites. The retained strength and modulus of all specimens that achieved run-out were evaluated. The presence of steam accelerated creep rates and reduced creep life of both CMCs. In the case of the composite with the aluminosilicate matrix, no-load exposure in steam at 1200 °C caused severe degradation of tensile strength. Composite microstructure, as well as damage and failure mechanisms were investigated. Poor creep performance of both composites in steam is attributed to the degradation of the fibers and densification of the matrix. Results indicate that the aluminosilicate matrix is considerably more susceptible to densification and coarsening of the porosity than the alumina matrix. The views expressed are those of the authors and do not reflect the official policy or position of the United States Air Force, Department of Defense or the U.S. Government.     

Effects of amines on the formation of β-ferric oxide hydroxide

Colloidal particles of -ferric oxide hydroxide (-FeOOH) were prepared by ageing an FeCl₃ solution at 100°C in the presence of various amines with different numbers of nitrogen atoms. The particle and crystallite sizes of the formed -FeOOH decreased with increasing concentration of amines, but the particles produced contained no amine. The influence of triethanolamine on the growth of -FeOOH particles was more marked than those of ethylenediamine, diethylenetriamine and triaminotriethylamine. The adsorption isotherms of nitrogen and water on the formed particles of different size were measured and surface fractal analysis was performed.     

Synthesis, characterization and oxide ionic conductivity of β-type solid solution in bismuth oxide doped with ytterbium oxide binary system

In this study, after doping Yb₂O₃ substance to α -Bi₂O₃ substance in the range of 1% ≤ n ≤ 8% in a series of different mole ratios, heat treatment was performed by applying a cascade temperature rise in the range of 700–790 °C for 48 and 120 h and new phases were obtained in the (Bi₂O₃)_1???x (Yb₂O₃) _x system. After 48 h of heat treatment at 750 °C and 120 h of heat treatment at 790 °C, mixtures containing 1–8% mole Yb₂O₃ formed a tetragonal phase. With the help of XRD, crystal systems and lattice parameters of the solid solutions were obtained and their characterization was carried out. Thermal measurements were made by using a simultaneous DTA/TG system. The total conductivity (σ _T) in the β-Bi₂O₃ doped with Yb₂O₃ system was measured using four-probe d.c. method.     

The influence of zinc oxide–cerium oxide nanoparticles on the structural characteristics and electrical properties of polyvinyl alcohol films

With the objective to investigate the influence of zinc oxide–cerium oxide (ZnO–Ce₂O₃) nanoparticles on the electrical properties of polyvinyl alcohol (PVA), PVA/ZnO–Ce₂O₃ nanocomposite films were prepared by solution intercalation method with different weight percentage viz., 0.5, 1.0, and 2.0?wt% of ZnO–Ce₂O₃ nanoparticles. The fabricated nanocomposites were characterized by Fourier transform-infrared spectroscopy (FT-IR), X-ray diffraction (XRD), and differential scanning calorimetry (DSC). The effect of ZnO–Ce₂O₃ nanoparticles on the dielectric constant (ε′), dielectric loss (ε″), electric modulus (M′ and M″), ac conductivity (σ _ac), and dielectric loss tangent (tan δ) over a range of frequencies at room temperature of PVA nanocomposites have been studied. FT-IR, XRD, and DSC analysis indicates the nature of ZnO–Ce₂O₃ nanoparticles interaction with the PVA matrix. The morphological behavior of the nanocomposites has been performed using scanning electron microscopy (SEM). The dielectric behaviors such as dielectric constant (ε′) and dielectric loss (ε″) increases with increase in nanoparticle concentration, but decreases with increase in frequency. But, the electric modulus (M′) increases with increase in frequency. Dielectric loss tangent (tan δ) decreases with increase in filler content at lower frequency, but at higher frequencies the tan δ increases with increase in nanoparticles content. AC conductivity (σ _ac) of PVA/ZnO–Ce₂O₃ nanocomposites increases with increasing frequency following the universal dielectric response law.     

The photo-electrochemical studies of Eu doped yttrium orthovanadate–zinc oxide–reduced graphene oxide nanohybrid

A new class of nanostructured photo-electrocatalyst Eu³⁺ doped yttrium orthovanadate–zinc oxide–reduced graphene oxide (YVO₄:Eu³⁺–ZnO–RGO) nanohybrid was developed by a simple electrostatic self-assembly at room temperature, using ZnO, YVO₄:Eu³⁺ and RGO as building blocks. Interaction among YVO₄:Eu³⁺, ZnO and RGO is indicated by variation in hydrodynamic diameter (H_D) and zeta potentials of the products as compared to their individual components, thus suggesting that YVO₄:Eu³⁺–ZnO–RGO is a nanohybrid and not a physical mixture. Electrochemical response of this nanohybrid towards the redox couple of Fe(CN)₆^3−/4− was investigated before and after UV irradiation. Apart from quenching of the green emission of ZnO in photoluminescence spectrum, which serves as a probe to monitor the interfacial electron transfer from excited ZnO to RGO, degradation in electrochemical redox process provides an additional path to monitor interfacial electron transfer.     

Magnetic properties and Mössbauer spectra of gamma ferric oxide and doped gamma ferric oxide

Magnetic hysteresis, Mössbauer spectra and temperature variation of initial magnetic susceptibility of thirteen samples of doped -Fe₂O₃ containing cobalt or gadolinium are determined. The samples containing more than 1.0% cobalt are found to have a multi-domain configuration, and undoped -Fe₂O₃, gadolinium-doped -Fe₂O₃ and doped -Fe₂O₃ containing less than 1.0% (except 0.3%) cobalt have a single domain configuration. Mössbauer spectra of gadoliniumdoped samples suggest that gadolinium occupies A and B sites. In cobalt-doped samples, the effective magnetic fields at A and B sites are different at room temperature and liquid nitrogen temperature. The samples which have a multi-domain configuration display an additional central doublet in Mössbauer spectra indicating that these samples contain multi-domain clusters. The saturation magnetization of gadolinium-doped -Fe₂0₃ is much lower, and the coercive force of cobalt-doped samples is much higher than of gadolinium-doped and undoped samples.     

Nanoscale epitaxial growth control of oxide thin films by laser molecular beam epitaxy—towards oxide nanoelectronics

The nanoscale growth control of oxide thin films, such as ferroelectric and magnetic materials, were explored by a novel technique based on nanoscale substrate engineering as well as atomic layer control via laser molecular beam epitaxy (laser-MBE). Atomic-scale analysis of the terminating layer of perovskite oxide films was performed by in situ coaxial impact-collision ion scattering spectroscopy. The novel heteroepitaxies that could be attained were: (1) the termination-regulated molecular layer-by-layer epitaxy of BaTiO₃ and La_0.7Sr_0.3MnO₃ thin films and (2) the step-decoration epitaxy resulting in the nanowire or nanodot structures of magnetic oxides such as (Mn, Zn) ferrite on ultrasmooth sapphire substrates with straight atomic steps.     

The effect of strontium oxide in glass–ionomer cements

The reaction of strontium oxide powder with poly(acrylic acid) has been studied both alone and within glass–ionomer cements. Reaction was found to be slow and the strontium-carboxylate structure was found to be partially covalent in character, as determined by Fourier transform infrared spectroscopy (FTIR). These are similar to the structures formed by calcium in glass–ionomer cements, but are different from typical monomeric strontium carboxylates, which tend to be purely ionic. Strontium oxide powder introduced in two types of glass–ionomer cements, slowed down the setting reaction at both 21 °C and 37 °C, but at low levels (5 wt %), increased the compressive strength in both cement formulations studied. However, at higher levels, it was found to decrease the compressive strength. This study confirms the view that strontium is a cement-forming ion; but concludes that, except at very low levels, strontium oxide powder does not improve the properties of glass–ionomer cements.     

Fine-tuning of stannic oxide anodes’ material properties through calcination

Journal of Materials Science: Materials in Electronics - Phase pure stannic oxide (SnO2) is an efficient and reliable anode material for Li ion batteries. Understanding of pure SnO2 phase formation...     

Preparation and characterization of epoxy/γ-aluminum oxide nanocomposites

Epoxy/γ-Al₂O₃ nanocomposites were prepared with a homogenizer and followed by a stepwise thermal curing process in this study. The dispersion of γ-Al₂O₃ nanoparticles was examined with a transmission electron microscopy (TEM). Meanwhile, the effects of γ-Al₂O₃ nanoparticles on thermal, dynamic mechanical and tensile properties of epoxy/γ-Al₂O₃ nanocomposites were also investigated and discussed. When the γ-Al₂O₃ content was increased from 1phr to 5phr, results revealed that γ-Al₂O₃ nanoparticles were effective to enhance both the stiffness and toughness of epoxy resin. Meanwhile, the maximum properties of glass transition temperature (T_g), T_d5%, storage modulus, tensile modulus, and elongation at break were observed in the epoxy/5phr γ-Al₂O₃ nanocomposite.     

Low-temperature synthesis of manganese oxide–carbon nanotube-enhanced microwave-absorbing nanocomposites

Noting that the dielectric properties of manganese oxide make it a promising microwave-absorbing material, a low-temperature method to deposit crystalline MnO₂ over carbon nanotubes (CNTs) is developed. Adjusting the pH of the precursor solution allows control over the phases and morphologies of the synthesized manganese oxides MnO₂ and Mn₃O₄ that have minimum reflection losses of ??11 dB and ??6 dB, respectively. The synthesized CNT–MnO₂ and CNT–Mn₃O₄ nanocomposites are superior microwave absorbers than simpler physical mixtures of CNTs and manganese oxides, with reflection losses as high as ??19 dB at 9.5 GHz and ??34 dB at 4 GHz, and have wider absorption bands than pure manganese oxides. Coating CNTs with manganese oxide not only increases dielectric and magnetic losses, but also improves the impedance match between free space and the absorber. The addition of CNTs to pure MnO₂ and Mn₃O₄ improves impedance matching by enhancing the relaxation polarization and conductivity losses, magnetic loss, including contributions form eddy current and natural resonance. This facile, low-cost, scalable, high-yield method produces an enhanced microwave-absorbing nanocomposite.     

Sol–gel synthesis and characterization of mesoporous manganese oxide

Mesoporous manganese oxide (MPMO) from reduction of KMnO₄ with maleic acid, was obtained and characterized in detail. The characterization of the material was confirmed by high-resolution transmission electron microscopy (HRTEM), X-ray powder diffractometry (XRD) and N₂ sorptometry. The results showed that MPMO is a pseudo-crystalline material with complex network pore structure, of which BET specific surface area is 297 m²/g and pore size distribution is approximately in the range of 0.7–6.0 nm. The MPMO material turns to cryptomelane when the calcinating temperature rises to 400 °C. The optimum sol–gel reaction conditions are KMnO₄/C₄H₄O₄ molar ratio=3, pH=7 and gelation time>6 h.     

Effect of Oxide Assisted Metal Nanoparticles on Microstructure and Morphology of Gallium oxide Nanowires

Several researches have been reported about the characteristic of β-Ga2O3 nanowires which was synthesized on nickel oxide particle. But indeed, recent researches about synthesis of β-Ga2O3 nanowires on oxide-assisted transition metal are limited to nickel or cobalt oxide catalyst. In this work, Gallium oxide (β-Ga2O3 ) nanowires were synthesized by a simple thermal evaporation method from gallium powder in the range of 700 - 1000℃ using the iron, nickel, copper, cobalt and zinc oxide as a catalyst, respectively. The β-Ga2O3 nanowires with single crystalline without defects were successfully synthesized at the reaction temperature of 850, 900 and 950℃ in all the catalysts. But optimum experimental condition in synthesis of nanowires varied with the kind of catalyst. As increasing synthesis temperature,the morphology of gallium oxide nanowires changed from nanowires to nanorods, and its diameter increased. From these results, we could be proposed that the growth mechanism of β-Ga2O3 nanowires was changed with synthesis temperature of nanowires. Microstructure and morphology of Synthesized nanowire was characterized by HR-TEM, FE-SEM, EDX and XRD.     

Enhanced capacitance of composite anodic ZrO₂ films comprising high permittivity oxide nanocrystals and highly resistive amorphous oxide matrix

Anodic oxide films with nanocrystalline tetragonal ZrO(2) precipitated in an amorphous oxide matrix were formed on Zr-Si and Zr-Al alloys and had significantly enhanced capacitance in comparison with those formed on zirconium metal. The capacitance enhancement was associated with the formation of a high-temperature stable tetragonal ZrO(2) phase with high relative permittivity as well as increased ionic resistivity, which reduces the thickness of anodic oxide films at a certain formation voltage. However, there is a general empirical trend that single-phase materials with higher permittivity have lower ionic resistivity. This study presents a novel material design based on a nanocrystalline-amorphous composite anodic oxide film for capacitor applications.     

An alternative route towards micro- and nano-patterning of oxide films

This paper presents a method to obtain submicron-?and nanometer structures of different oxide films and heterostructures combining e-beam lithography and chemical etching. The most relevant advantage of this method is that structures of tens of microns in length and below ～100?nm width can be produced, keeping the intrinsic bulk film properties, as proven by electrical transport measurements. In this way our method provides a bridge that connects the attractive properties of oxide films and the nanoworld.     

Preparation and magnetic characteristics of mesoporous nickel oxide–silica composites

Mesoporous NiO–SiO₂ (MCM-41) silica-matrix composites with various nickel oxide concentrations (NiO : SiO₂ = 0.025 : 1 to 0.2 : 1) have been produced by oxide cocondensation under hydrothermal synthesis conditions in the presence of cetyltrimethylammonium bromide as a template and (2-cyanoethyl) triethoxysilane as an organosubstituted trialkoxysilane additive. X-ray diffraction data have been used to evaluate the maximum nickel(II) oxide concentration (NiO : SiO₂ = 0.1 : 1) that allows the ordered mesopore structure of MCM-41 to persist in the silica-matrix composites. We have studied the magnetic properties of this material as functions of temperature and magnetic field. The results demonstrate that the magnetic properties of the nanocomposite with NiO : SiO₂ = 0.1 : 1 at low temperatures (T < 20 K) are determined by incomplete spin compensation in the matrix and on the surface of the NiO nanoparticles.     

Metallic and insulating interfaces of amorphous SrTiO₃-based oxide heterostructures

The conductance confined at the interface of complex oxide heterostructures provides new opportunities to explore nanoelectronic as well as nanoionic devices. Herein we show that metallic interfaces can be realized in SrTiO(3)-based heterostructures with various insulating overlayers of amorphous LaAlO(3), SrTiO(3), and yttria-stabilized zirconia films. On the other hand, samples of amorphous La(7/8)Sr(1/8)MnO(3) films on SrTiO(3) substrates remain insulating. The interfacial conductivity results from the formation of oxygen vacancies near the interface, suggesting that the redox reactions on the surface of SrTiO(3) substrates play an important role.     

Sintering of Al–Zr based oxide ceramics using thermal plasma

A novel and low cost extended arc thermal plasma heating (EATPH) reactor [Roul et al., JMSP 6 (1) (1998)] has been used to sinter Al–Zr oxide ceramics within a few minutes in Ar atmosphere instead of a few tens of hours by conventional furnace heating. Critical experimental parameters such as plasma power (kW), plasmagen gas flow rate, sintering time and electrode spacing distance are optimized to achieve high density sintered materials. It is noted that sintering time is approximately reciprocal to plasma power. Higher plasma power with less sintering time can generate high-density homogeneous material without significant grain growth. XRD and SEM studies were carried out to characterize and evaluate the sintered materials. Surface morphology revealed uniform particle size distribution in long-range order, with no runway grain growth during this EATPH sintering process. This simple EATPH method provides an alternative and quick technique for tailoring high temperature ceramic materials over conventional sintering method due to fast heat and mass transfer kinetics inside thermal plasma reactor.