Crystallization behaviour and high coercivity of （Nd,Pr）（13）Fe（80）Nb1B6 melt-spun ribbons

Amorphous (Nd,Pr)₁₃Fe₈₀Nb₁B₆ ribbons were crystallized at 670–730°C for 5–25 min to study the effects of isothermal crystallization on their behavior and magnetic properties. XRD results indicate that the isothermal incubation time is 12, 5, and less than 5 min at 670, 700, and 730°C, respectively. High coercivities, with the maximum value of _i H _c = 1616 kA/m at 700°C for 19 min, measured by a physical property measurement system, are obtained in the crystallized ribbons. This is mainly attributed to the addition of Pr and Nb, because Pr₂Fe₁₄B has a higher anisotropic field than Nd₂Fe₁₄B, and Nb enriched in the grain boundary regions can not only reduce the exchange-coupling effects among hard grains, but also impede grain growth during the crystallization process. In addition, it should also be related to the characteristics of the furnace that the authors designed.     

Thermoelectric properties of n-type Bi<Subscript>2</Subscript>Te<Subscript>2.7</Subscript>Se<Subscript>0.3</Subscript> compounds prepared by spark plasma sintering

In this study, the thermoelectric properties of 0.1 wt.% Cdl₂-doped n-type Bi₂Te_2.7Sb_0.3 compounds, fabrieated by SPS in a temperature range of 250°C to 350°C, were characterized. The density of the compounds was increased to approximately 100% of the theoretical density by carrying out consolidation at 350°C. The Seebeck coefficient, thermal conductivity, and electrical resistivity were dependent on a hydrogen reduction process and the sintering temperature. The Seebeck coefficient and the electrical resistivity increased with the reduction process. Also, electrical resistivity decreased and thermal conductivity increased with sintering temperature. The results suggest that carrier density and mobility vary according to the reduction process and sintering temperature. The highest figure of merit, 1.93×10⁻³ K⁻¹, was obtained for the compound consolidated at 350°C for 2 min.     

Preparation of ultra-fine FeNiMnO<Subscript>4</Subscript> powders and ceramics by a solid-state coordination reaction

A mixed oxalate FeNiMn(C₂O₄)₃·nH₂O, a coordination compound, was synthesized by milling a mixture of ferrous iron chloride, nickel acetate, manganese acetate, and oxalic acid at room temperature. A spinel-structured FeNiMnO₄ powder with high sintering activity and chemical homogeneity was obtained by calcining the mixed oxalate in air at 800°C for 2 h. Dense FeNiMnO₄ ceramics with a relative density of ∼98% were achieved by sintering powder compacts at a lower temperature of 1100°C for 5 h. The specific resistivityρ _25°C and the thermal constant B_25/85°C were 4382 Ω·cm and 3373 K, respectively. The aging coefficient ΔR/R(%) of the ceramics after annealing at 150°C for 500 h was 0.6%.     

Dielectric properties of ZrTiO<Subscript>4</Subscript> thin films synthesized by sol-gel method

ZrTiO₄ thin films were successfully prepared on Pt/Ti/SiO₂/Si(100) substrates by a sol-gel process and gel films were heat-treated at various temperatures. The surface morphology, crystal structure, and dielectric properties of the thin films were investigated. It was possible to obtain ZrTiO₄ phase at temperatures above 650 °C for 2 h, which is much lower than the bulk sintering temperature. The microstructure of well-crystallized ZrTiO₄ thin films was a fine-grained microstructure less than 70 nm in grain size and the surface morphology was smooth with 22.4 rms roughness. The dielectric constant and loss of ZrTiO₄ thin films were 38 and 0.006, respectively, for thin films with 450 nm thickness heat-treated at 900 °C for 2 h.     

Microstructure and hot deformation behavior of A356/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composite fabricated by infiltration method

The hot deformation behavior of an A356/Al₂O₃ composite fabricated by the infiltration method was characterized in the temperature range of 300-500 °C and strain rate range of 0.001-1/s using compressive tests. The composite consists of an Al-Si based matrix and nano-sized Al₂O₃ particulates. A constitutive model was established based on the hyperbolic sine Arrhenius type equation and its hot workability was evaluated by means of processing maps based on Dynamic Material Modeling. The activation energy for hot deformation was calculated to be 223 kJ/mol, which is higher than the activation energy for self-diffusion of pure aluminum (142 kJ/mol). The optimum processing condition for the hot working of the composite was found to exist at 500 °C with a strain rate of 1/s, where a dynamic recrystallized microstructure was observed and the maximum efficiency was exhibited in the processing map. Voids were frequently detected at 500 °C with lower strain rates, deteriorating the workability of the composite.     

Suspension Plasma-Sprayed ZnFe<Subscript>2</Subscript>O<Subscript>4</Subscript> Nanostructured Coatings for ppm-Level Acetone Detection

Zinc ferrite (ZnFe₂O₄) sensitive coatings have been deposited by suspension plasma spraying. The phase constitution of the coatings was characterized by x-ray diffraction while the top surface and cross-sectional morphology of the coatings were inspected by scanning electron microscopy. The response to acetone was tested with the concentration in the range of 25-500 ppm at the working temperature from 175 to 275 °C. The sensors that were deposited at an arc current of 400 A showed better performance than those at 600 A owing to small grain size and high porosity. The sensor response increased with acetone concentration. The optimized sensors showed excellent response/recovery time and selectivity to acetone at 200 °C.     

Preparation of CuInSe<Subscript>2</Subscript> films by ultrasonic electrodeposition-selenization and the improvement of their surface morphology

The CuInSe₂ compound was prepared by selenization of Cu-In precursor, which was ultrasonic electrodeposited at constant current. CuInSe₂ films were compacted to improve surface morphology. The films were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS). It is indicated that ideal stoichiometric CuInSe₂ films can be obtained by the selenization of Cu-In precursor deposited at a current density of 20 mA/cm². Single-phase CuInSe₂ is formed in the selenization process, and it exhibits preferred orientation along the (112) plane. The CuInSe₂ films with smooth surface can be obtained under the pressure of 500 MPa at 60°C.     

Hetero-Orientation Epitaxial Growth of TiO<Subscript>2</Subscript> Splats on Polycrystalline TiO<Subscript>2</Subscript> Substrate

In the present study, the effect of titania (TiO₂) substrate grain size and orientation on the epitaxial growth of TiO₂ splat was investigated. Interestingly, the splat presented comparable grain size with that of substrate, indicating the hereditary feature of grain size. In addition, hetero- and homo-orientation epitaxial growth was observed at deposition temperatures below 400 °C and above 500 °C, respectively. The preferential growth of high-energy (001) face was also observed at low deposition temperatures (≤?400 °C), which was found to result from dynamic nonequilibrium effect during the thermal spray deposition. Moreover, thermal spray deposition paves the way for a new approach to prepare high-energy (001) facets of TiO₂ crystals.     

Microstructures and Properties of Nanostructured TiN/MoS<Subscript>2</Subscript>/Ag Composite Film Prepared by Pulsed Laser Deposition

In this work, the structural and mechanical properties, tribological performance, and lubrication mechanism from room temperature to 900 °C of TiN/MoS₂/Ag composite films were investigated in detail. Nanostructured TiN/MoS₂/Ag composite film was obtained by assembling targets using pulsed laser deposition. The incorporation of lubricant layered MoS₂ and soft metal Ag led to degraded mechanical properties, which could contribute to the lower friction coefficients at low temperatures. When the temperature increased to above 500 °C, the generated high-temperature lubricant MoO₃ and silver molybdates played a critical synergetic lubrication effect, which formed a layer of lubricating film and reduced the friction coefficient. Thus, the cooperation of various lubrication phases contributed to improvement of tribological performance and resulted in continuous lubrication from room temperature to 900 °C.     

Rate of FeO Reduction from a CaO-SiO<Subscript>2</Subscript>-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> Slag by Carbon-Saturated Iron

Reaction rates have been measured for the reduction of FeO from a lime-silica-alumina slag over carbon-saturated iron in graphite crucibles. The initial FeO concentrations were under 5 pet in a base slag composition of 46 to 47 pet CaO, 38 to 39 pet SiO₂, 15 to 16 pet A1₂O₈.The reaction rate was found to be proportional to about the second power of the analyzed iron content of the slag. Two rate constants were obtained for simultaneous reactions at the slag-metal and slag-graphite interfaces. Values for these constants at 1430°C (2606°F) were k₁ = 0.00058 g FeO per (min) (sq cm) (pet FeO)² at the metal and k₂ = 0.00012 (same dimensions) at the graphite. The temperature coefficient was not measured independently for the two reactions, but the net effect of a 140°C rise in temperature was small.Iron droplets rose to the surface of the slag with gas bubbles and collected in a ring adjacent to the crucible wall in amount equal to or greater than the weight of iron calculated from FeO reduction, in those runs with both slag and metal. When only slag was present in the crucible, the iron beads were more evenly distributed over the entire crucible wall and were smaller in size and total amount.It is not possible to deduce a reaction mechanism to interpret the observations on the basis of these experiments alone, but several alternatives have been discussed in terms of intermediate reaction products, dissociation of FeO in the slag, diffusion, nucleation of gas or metal, and surface phenomena leading to reaction through iron films on rising bubbles of CO in the slag.The rate of reduction of FeO in the absence of sulphur is qualitatively consistent with the part that this reaction is believed to play in the desulphurization of iron by slags under similar experimental conditions.     

Preparation of High Purity ZrCl<Subscript>4</Subscript> from Alkali Chlorozirconates

High purity ZrCl₄ (25 to 200 ppm of metallic impurities) can be readily prepared in simple apparatus by thermal decomposition of alkali chlorozirconate fused salts at 500° to 600°C and at atmospheric pressure. Suggested phase diagrams for the systems NaCl-ZrCl₄ and KCl-ZrCl₄ are presented.     

Tunneling magnetoresistance in sintered Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> samples diluted with Fe and α-Fe<Subscript>2</Subscript>O<Subscript>3</Subscript>

Electric transport and magnetoresistance characteristics were investigated for Fe₃O₄-x Fe(x=0, 10, 20 wt.%) samples and Fe₃O₄-α-Fe₂O₃ samples sintered at 500°C. For composition dependence of Fe₃O₄-x Fe samples, the largest room temperature MR, 3.3% at 10 kOe, was obtained from a Fe₃O₄-10 Fe sample. For the surface heat treatment dependence of Fe₃O₄ powders, the largest room temperature MR, 4% at 10 kOe, was obtained from a Fe₃O₄-α-Fe₂O₃ sample sintered with Fe₃O₄ powders heated at 200°C in air. It was found that these enhanced MR ratios always appear together with the appropriate excess resistance which is regarded as the tunneling barrier. These enhanced MR ratios of Fe₃O₄-10 Fe and Fe₃O₄-α-Fe₂O₃ samples can be explained by the increased interparticle contact sites and the appropriate thickness of α-Fe₂O₃, respectively.     

Properties of nickel-cobalt composite silicides by thermal annealing of Ni<Subscript>1−x</Subscript>Co<Subscript>x</Subscript> (x=0.2, 0.5, and 0.8) alloy thin films on silicon and polysilicon substrates

10 nm-Ni_1−xCo_x (x=0.2, 0.5, and 0.8)/p-Si(100)(or poly crystalline Si) was thermally annealed using rapid thermal annealing for 40 s at 600–1100°C. The annealed film structures developed into NiCoSi_x, and the resulting changes in sheet resistance, microstructure, and composition were investigated using a four-point probe, a scanning electron microscope, a field ion beam, an X-ray diffractometer, and an Auger electron spectroscope. The final thickness of NiCoSi_x formed on single-crystal silicon was approximately 12.64nm, and it maintained its sheet resistance below 20 Ω/sq. during the silicidation annealing at 1100°C. The NiCoSi_x formed on polysilicon had a thickness of 35.04nm, and its low resistance was maintained up to 900°C. Additional annealing of silicides at the given RTA temperature for 30 min resulted in a drastic increase in sheet resistance. We identified Ni₃Si₂ and a NiSi phase at 700°C and 1000°C for single-crystal silicon substrates. Moreover, Ni₃Si₂, NiSi, and CoSi₂ phases were stable at 700°C, and then NiSi₂ and Ni₃Si₂ became stable for polycrystalline silicon substrates at 1000°C. When the amount of Co was 80%, only a Ni₃Si₂ phase was confirmed at 700°C and 1000°C in both the single and polycrystalline substrates. With less Co (Co=0.2, 0.5), Ni₃Si₂, NiSi, and CoSi₂ phases were observed at 700, and Ni₃Si₂ and NiSi₂ phases were observed at 1000°C. Cobalt also improved thermal stability of the silicides formed on the polysilicon gate, but this enhancement was lessened due to the silicon mixing during high temperature diffusion. In conclusion, the proposed nickel cobalt composite silicides formed from the nano-thick alloy films may be superior to conventional nickel monosilicides due to improved thermal stability.     

Recovery of V<Subscript>2</Subscript>O<Subscript>5</Subscript> from Bayer liquor by ion exchange

A new technology was developed to recover V2O5 from Bayer spent liquor by ion exchange.The experimental results show that in the conditions of 105°C and 0.20-0.25 mass ratios between CaO in lime and Al2O3 in spent liquor, the precipitation rate of vanadium in Bayer liquor is more than 85%.The vanadium-bearing precipitation is leached by NaHCO3 solution.The leaching rate of vanadium can reach 85% in the conditions of 95°C, 40 g·L-1 of NaHCO3 concentration, and ventilating of CO2.The 201 × 7 type of resin has...     

Phase Formation of the Yttrium Aluminates in the Y<Subscript>2</Subscript>O<Subscript>3</Subscript>-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-SiC System

Phase formation sequence of the yttrium aluminates in the Y₂O₃-Al₂O₃-SiC ternary system as temperature increases were investigated via x-ray diffraction (XRD). Results showed that YAM (monoclinic), YAP (perovskite) and YAG (garnet) were the yttrium aluminates presented in the solid-state reacted samples at a fixed Al₂O₃:SiC ratio of 1:1. Formation of the yttrium aluminates depended on the temperature. The YAM, YAP and YAG started to form below 1150 °C, at 1300 °C, and at 1450 °C, respectively. Accordingly, two behavior phase diagrams of the Y₂O₃-Al₂O₃-SiC ternary system were recognized, one is in the temperature range of 1150-1300 °C and the other is in 1300-1450 °C, respectively. Thereafter, the phase equilibrium was reached in the temperature range of 1450-1700 °C. Effects of SiC on the phase formation processes in the ternary system were discussed.     

Synthesis and Characterization of New Bismuth Lead Vanadate Pb<Subscript>2</Subscript>BiV<Subscript>3</Subscript>O<Subscript>11</Subscript>

It has been shown that BiVO₄ and Pb₂V₂O₇ react with each other, forming a new compound of the formula Pb₂BiV₃O₁₁ at molar ratio equal to 1:1. This compound has also been obtained from PbO, Bi₂O₃, and V₂O₅, mixed at a molar ratio of 4:1:3. It melts congruently at a temperature of 725 ± 5 °C and crystallizes in the triclinic system with unit-cell parameters: a = 0.710076 nm, b = 1.41975 nm, c = 1.42972 nm, α = 134.552°, β = 97.2875°, γ = 89.6083°, and Z = 4.     

Multiferroic BiFeO<Subscript>3</Subscript> thick film fabrication by aerosol deposition

BiFeO₃ (BFO) multiferroic materials in the crystalline phase require very delicate processing conditions. In order to fabricate a high quality BFO thick film, aerosol deposition (AD) was employed and the phase evolution and multiferroic properties of the film were investigated for different annealing temperatures. A BFO thick film annealed at 500 °C had a dielectric constant of 80 at 1 kHz and possessed ferroelectric characteristics. At an applied electric field of ∼900 kV/cm, the remaining polarization and coercive field (E_c) were approximately 7.5 μC/cm² and 370 kV/cm, respectively. In addition, the BFO thick film fabricated via AD and annealed at 500 °C showed weak ferromagnetic behavior between −1250 Oe and +1250 Oe and was saturated at the higher magnetic field strength, showing ferromagnetic behavior.     

Fabrication of TiSi<Subscript>2</Subscript> using microwave hydrogen plasma annealing

A new method, microwave hydrogen plasma annealing of sputter-deposited titanium films on an Si (111) substrate, was used to fabricate TiSi₂ films. The films were characterized by x-ray diffraction, Auger electron spectroscopy, sputter depth profiling, and four-point probe resistivity measurements. Polycrystalline TiSi₂, dominated by components with (040) orientation, was grown at the annealing temperature of 800 °C. The microwave hydrogen plasma was considered not only to provide the heat for the solid-phase reaction, but also to promote the solid-phase reaction by enhancing atom mobility and diffusion.     

Effects of defects generated in ALD TiO<Subscript>2</Subscript> films on electrical properties and interfacial reaction in TiO<Subscript>2</Subscript>/SiO<Subscript>2</Subscript>/Si system upon annealing in vacuum

Thin TiO₂ layers grown at 130°C on SiO₂-coated Si substrates by atomic layer deposition (ALD) using TTIP and H₂O as precursors were annealed, and the effects of the annealing temperature on the resulting electrical properties of TiO₂ and the interface properties between a Pt electrode and TiO₂ were examined using transmission line model (TLM) structures. The as-deposited TiO₂ thin film had an amorphous structure with OH groups and a high resistivity of 6×10³Ω-cm. Vacuum annealing at 700 °C transformed the amorphous film into an anatase structure and reduced its resistivity to 0.04Ω-cm. In addition, the vacuum-annealing of the TiO₂/SiO₂ structure at 700°C produced free silicon at the TiO₂-SiO₂ interface as a result of the reaction between the Ti interstitials and SiO₂. The SiO₂ formed on the TiO₂ surface caused a Schottky contact, which was characterized by the TLM method. The use of the TLM method enabled the accurate measurement of the resistivity of the vacuum-annealed TiO₂ films and the characterization of the Schottky contacts of the metal electrode to the TiO₂.     

Evaluation of in vitro and in vivo tests for surface-modified titanium by H<Subscript>2</Subscript>SO<Subscript>4</Subscript> and H<Subscript>2</Subscript>O<Subscript>2</Subscript> treatment

Titanium is widely used as an implant material for artificial teeth. Furthermore, various studies have examined surface treatment with respect to the formation of a fine passive film on the surface of commercial titanium and its alloys and to improve the bioactivity with bone. However, there is insufficient data about the biocompatibility of implant materials in the body. The purpose of this study was to examine whether surface modification affects the precipitation of apatite on titanium metal. Specimens were chemically washed for 2 min in a 1∶1∶1.5 (vol.%) mixture of 48 %HF, 60%HNO₃ and distilled water. The specimens were then chemically treated with a solution containing 97%H₂SO₄ and 30%H₂O₂ at the ratio of 1∶1 (vol.%) at 40°C for 1h, and subsequently heat-treated at 400°C for 1h. All the specimens were immersed in HBSS with pH 7.4 at 36.5°C for 15d, and the surface was examined with TF-XRD, SEM, EDX and XPS. In addition, specimens of commercial pure Ti, with and without surface treatment, were implanted in the abdominal connective tissue of mice for 28 d. Conventional aluminum and stainless steel 316L were also implanted for comparison. An amorphous titania gel layer was formed on the titanium surface after the titanium specimen was treated with a solution of H₂SO₄ and H₂O₂. The average roughness was 2.175 μm after chemical surface treatment. The amorphous titania was subsequently transformed into anatase by heat treatment at 400°C for 1h. The average thickness of the fibrous capsule surrounding the specimens implanted in the connective tissue was 47.1μm in the chemically treated Ti, and 52.2, 168.7 and 101.9μm, respectively, in the untreated commercial pure Ti, aluminum and stainless steel 316L.