Low Solution Temperature Heat Treatment of AlSi<Subscript>9</Subscript>Cu<Subscript>3</Subscript>(Fe) High-Pressure Die-Casting Actual Automotive Components

Usually, high-pressure die-casting (HPDC) components cannot be heat-treated at high temperature without the occurrence of surface blisters, which are unacceptable for surface finish and may reduce the mechanical properties. In this context, the purpose of the present paper was to analyze the effectiveness of special low solution temperature T6 heat treatment in overcoming this limit for HPDC AlSi₉Cu₃ alloy. Very low solution temperatures (<?450 °C, followed by 165 °C aging) to prevent the occurrence of blisters were combined with commonly used times (from 1 to 16 h) ensuring the feasibility of industrial application. Treatments were conducted on samples extracted from actual castings to evaluate the typical defects encountered in common production. Properties were analyzed by means of visual inspection, microstructural observations, image analysis, hardness, tensile tests and fractography. The results showed that it is possible to use solubilization temperatures below 450 °C for several hours in a T6 treatment to give strengthening without relevant blistering in AlSi₉Cu₃ alloy. The optimum match of properties was provided by a solution treatment at 430 °C for 4 h followed by an aging at 165 °C for 8 h, which gave a yield increase of ~?50 MPa, an increase in ductility and the best Quality Index value.     

Formation of high-density TiN/Ti<Subscript>5</Subscript>Si<Subscript>3</Subscript> ceramic composites using preceramic polymer

The formation, microstructure and properties of high-density TiN/Ti₅Si₃ ceramic composites created by the pyrolysis of preceramic polymer with filler were investigated. Methylpolysiloxane was mixed with TiH₂ as filler and ceramic composites prepared by pyrolysis at 1200°C to 1600°C under N₂, Ar and vacuum were studied. When a specimen with 70 vol.% TiH₂ was pyrolyzed up to 1600°C in a vacuum after a preheat treatment at 850°C in a N₂ atmosphere and subsequently heat-treated at 1600°C for 1 h under Ar at a pressure of 2 MPa, a ceramic composite with full density was obtained. The microstructure of the ceramic composite was composed of TiN and Ti₅Si₃ phases. Under specific pyrolysis conditions, a ceramic composite with a density of 99.2 TD%, a Vickers hardness of 18 GPa, a fracture toughness of 3.5 MPam^1/2, a flexural strength of 270 MPa and a electrical conductivity of 6200 ohm⁻¹·cm⁻¹ was obtained.     

Mechano-thermal treatment of TiO<Subscript>2</Subscript>-Al powder mixture to prepare TiAl/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composite

In this research, a composite comprising an intermetallic matrix and dispersed Al₂O₃ particles was processed. A mixture of TiO₂ and Al was mechanically activated in the presence of a process control agent and/or without it, in a high-energy planetary ball mill. As a subsequent process, the sample was sintered at various temperatures. The phase composition and morphology of the samples were evaluated by XRD and SEM techniques, respectively. The thermal behavior of the samples milled for 8 h with PVA and/or without it, were also assessed by the DTA technique and compared with one another. The DTA results revealed that addition of PVA shifted the aluminothermic reduction of TiO₂ to higher temperatures; therefore, final composite phases were developed at higher temperatures. The results also showed that addition of PVA during milling caused the final microstructure to coarsen. The XRD pattern of the sample sintered at 700 °C exhibits the existence of TiAl, Ti₃Al, and Al₂O₃ phases. In the sample sintered at 850 °C, the remaining Ti₃Al peak was attenuated and completely disappeared at 1000 °C.     

Temperature dependent surface morphology and lithium diffusion kinetics of LiCoO<Subscript>2</Subscript> cathode

In an attempt to understand the effect of synthesis temperature upon surface morphology and lithium diffusion kinetics of LiCoO₂, the compound was synthesized at four different temperatures, viz., 600, 700, 800 and 900 °C using a novel gelatin-assisted combustion method. LiCoO₂ synthesized at 800 °C is found to be a mixture of rhombohedral and cubic LiCoO₂ and a temperature of 900 °C leads to the formation of cubic LiCo₂O₄ compound, thus favoring lower temperatures such as 600 and 700 °C to prepare phase pure rhombohedral LiCoO₂. Cyclic voltametry and impedance spectral studies evidence that LiCoO₂ synthesized at 600 °C exhibits better electrochemical cycling behavior and considerably reduced internal resistance upon cycling, which are substantiated further from the higher lithium diffusion coefficient value. The study demonstrates the possibility and superiority of synthesizing electrochemically active LiCoO₂ with preferred surface morphology and better lithium diffusion kinetics at a relatively lower temperature of 600 °C, using a gelatin-assisted combustion method.     

Physicochemical Properties of Spray-Deposited CoFe2O4 Thin Films

Cobalt ferrite thin films are deposited onto quartz glass substrates by chemical spray pyrolysis technique at different substrate temperatures using ferric nitrate and cobalt nitrate as precursors. Thermogravimetric analysis (TGA) study indicates the formation of CoFe₂O₄ by decomposition of cobalt and ferric nitrates after 800 °C. X-ray diffraction studies reveal that annealed films are polycrystalline in nature and exhibit spinel cubic crystal structure. Crystallite size varies from 39 to 44 nm with the substrate temperatures. Direct optical band gap energy of CoFe₂O₄ thin films is found to be 2.57 eV. The AFM images show that roughness and grain size of the CoFe₂O₄ thin film are about 9 and 138 nm, respectively. The measured DC resistivity of the deposited thin films indicates that as temperature increases the resistivity decreases indicating the semiconductor nature of the films. Decrease in dielectric constant (ε′) and loss tangent (tanδ) has been observed with frequency and attains the constant value at higher frequencies. The AC conductivity of cobalt ferrite thin films increases with increase in frequency. Thus, the prepared films show normal dielectric performance of the spinel ferrite thin film. Room-temperature complex impedance spectra show the incomplete semicircles as films exhibit high resistance values at lower frequencies.     

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.     

Control of microwave dielectric properties in 0.42ZnNb<Subscript>2</Subscript>O<Subscript>6</Subscript>−0.58TiO<Subscript>2</Subscript> ceramics by the quantitative analysis of phase transition

Phase constitutions of ZnNb₂O₆−TiO₂ mixture ceramics were significantly changed according to the sintering temperature. Phase transition procedures and their effect on the microwave dielectric properties of 0.42ZnNb₂O₆−0.58TiO₂ were investigated using X-ray powder diffraction and a network analyzer. The fractions of the phases composing the mixture were calculated by measuring integral intensities of each reflection. The structural transitions in 0.42ZnNb₂O₆−0.58TiO₂ were interpreted as the association of two distinct steps: the columbite and rutile to ixiolite transition present at lower temperatures (900–950°C) and the ixiolite to rutile transition at higher temperatures (1150–1300°C). These transitions caused considerable variation of microwave dielectric properties. Importantly, τ_f was modified to around 0 ppm/°C in two sintering conditions (at 925°C for 2 hr and at 1300°C for 2 hr), by the control of phase constitution.     

Reaction Time and Film Thickness Effects on Phase Formation and Optical Properties of Solution Processed Cu<Subscript>2</Subscript>ZnSnS<Subscript>4</Subscript> Thin Films

Copper-zinc-tin-sulfide (Cu₂ZnSnS₄ or CZTS) is a promising p-type semiconductor material as absorber layer in thin film solar cells. The sulfides of copper and tin as well as zinc and sulfur powders were dissolved in hydrazine. The effect of chemical reaction between precursor species, at room temperature, was assessed for 6 to 22 h. For 22 h reaction time, the effect of spin coated film thickness on the resulting composition, after annealing under N₂ flow at 500 °C for 1 h, was investigated. The morphology, composition, and optical properties of the annealed films were determined by means of x-ray diffraction, scanning electron microscope, and spectrophotometer studies. It was found that, for less than optimal reaction time of 22 h or film thickness below 1.2 µm, other ternary phases namely Cu₄SnS₄, Cu₅Sn₂S₇, and ZnS co-exist in different proportions besides CZTS. Formation of phase-pure CZTS films also exhibited a tendency to minimize film cracking during annealing. Depending on the processing conditions, the band gap (E _g) values were determined to be in the range of 1.55 to 1.97 eV. For phase-pure annealed CZTS film, an increase in the E _g value may be attributed to quantum confinement effect due to small crystallite size.     

Facile synthesis,morphology and structure of Dy<Subscript>2</Subscript>O<Subscript>3</Subscript> nanoparticles through electrochemical precipitation

The aim of this research was to introduce a new, facile and simple method for synthesis of Dy₂O₃ nanostructures at room temperature. For the first time, galvanostatic electrodeposition was used to synthesize Dy₂O₃ particles, and the influence of the current density on the structure and morphology of the product was studied. The samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and Brunauer–Emmett–Teller (BET). The results show that the current density has little effect on the chemical composition but great effect on the structure and morphology of the samples. The average size of the particles decreases as the applied current density increases. The grain size of as-prepared samples decreases from 500 to 70 nm when the current density increases from 0.5 to 6.0 mA·cm^?2. To obtain oxide product, the as-prepared samples were heat-treated at 1,000 °C. The results show that the heat-treated samples have smaller particles. The XRD results show that the similar patterns are observed in the samples synthesized at different current densities, and the only difference from the JCPDS card is the ratio of peak intensities. With the increase in the current density, a decrease in the current efficiency is observed.     

Characterization of rapid thermally processed LiMn204 thin films derived from solution deposition

Cathode material LiMn₂O₄ thin films were prepared through solution deposition followed by rapid thermal annealing. The phase identification and surface morphology were studied by X-ray diffraction and scanning electron microscopy. Electrical and electrochemical properties were examined by four-probe method, cyclic voltammetry and galvanostatic charge-discharge experiments. The results show that the film prepared by this method is homogeneous, dense and crack-free. As the annealing temperature and annealing time increase, the electronic resistivity decreases, while the capacity of the films increases generally. For the thin films annealed at different temperatures for 2 min, the thin film annealed at 800 °C has the best cycling behavior with the capacity loss of 0.021% per cycle. While for the thin films annealed at 750 °C for different times, the film annealed for 4 min possesses the best cycling performance with a capacity loss of 0.025% per cycle. For the lithium diffusion coefficient in LiMn₂O₄ thin film, its magnitude order is 10⁻¹¹ cm²·s⁻¹.     

Dielectric properties of Ta<Subscript>2</Subscript>O<Subscript>5</Subscript> thin films deposited onto Ti and TiO<Subscript>2</Subscript> layer

The present study describes the dielectric properties of RF sputtered Ta₂O₅ thin films as a function of the buffer layer and annealing condition. The buffer layers were Ti or TiO₂. And the thin film was annealed in various conditions. The X-ray pattern results showed that the phase of the RF sputtered Ta₂O₅ thin films was amorphous and this state was kept stable to RTA (rapid thermal annealing) even at 700°C. Measurements of the electrical and dielectric properties of the reactive sputtered Ta₂O₅ fabricated in two simple metal insulator semiconductor (MIS) structures, (Cu/Ta₂O₅/Ti/Si/Cu and Cu/Ta₂O₅/TiO₂/Si/Cu) indicated that the amorphous Ta₂O₅ grown on Ti possesses a high dielectric constant (30–70) and high leakage current (10⁻¹–10⁻⁴ A/cm²), whereas a relatively low dielectric constant (−10) and low leakage current (−10⁻¹⁰ A/cm²) were observed in the amorphous Ta₂O₅ deposited on the TiO₂ buffer layer. In addition, the leakage current mechanisms of the two amorphous Ta₂O₅ thin films were investigated by plotting the relation of current density (J) vs. applied electric field (E). The Ta₂O₅/Ti film exhibited three dominant conduction mechanism regimes contributed by the Ohmic emission at low electrical field, by the Schottky emission at intermediate field and by the Poole-Frenkel emission at high field. In the case of Ta₂O₅/TiO₂ film, the two conduction mechanisms, the Ohmic and Schottky emissions, governed the leakage current density behavior. The conduction mechanisms at various electric fields applied were related to the diffusion of Ta, Ti and O, followed by the creation of vacancies, in the rapid thermal treated capacitors.     

Preparation and dielectric properties of compositionally graded （Ba, Sr）TiO3 thin film by sol-gel technique

Compositional graded BaxSr1-xTiO3 （x=0.6, 0.7, 0.8, 0.9, 1.0） （BST） thin films （less than 400 nm） were fabricated on Si and Pt/Ti/SiO2/Si substrates by sol-gel technique. A special heating treatment was employed to form the uniform composition gradients at 700 ℃. The microstructures of the films were studied by means of X-ray diffraction, atomic force microscope and field emission scanning electron microscopy. The results show that the films have uniform and crack-free surface morphology with perovskite structure phase. The small signal dielectric constant （εr） and dielectric loss （tanδ） are found to be 335 and 0.045 at room temperature and 200 kHz. The dielectric properties change significantly with applied dc bias, and the graded thin film show high tunability of 42.3% at an applied field of 250 kV/cm. All the results indicate that the graded BST thin films prepared by sol-gel technique have a promising candidate for microelectronic device.     

Preparation and characterization of nanostructured Bi<Subscript>2</Subscript>Se<Subscript>3</Subscript> and Sn<Subscript>0.5</Subscript>-Bi<Subscript>2</Subscript>Se<Subscript>3</Subscript>

Nanostructured Bi₂Se₃ and Sn_0.5-Bi₂Se₃ were successfully synthesized by hydrothermal coreduction from SnCl₂·H₂O and the oxides of Bi and Se. The products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and field emission scanning electron microscope (FESEM). Bi₂Se₃ powders obtained at 180°C and 150°C consist of hexagonal flakes of 50–150 nm in side length and nanorods of 30–100 nm in diameter and more than 1 μm in length. The product obtained at 120°C is composed of thin irregular nanosheets with a size of 100–200 nm and several nanometers in thickness. The major phase of Sn_0.5-Bi₂Se₃ synthesized at 180°C is similar to that of Bi₂Se₃. Sn_0.5-Bi₂Se₃ powders are primarily nanorod structures, but small amount of powders demonstrate irregular morphologies.     

Precipitation of Secondary Carbides in M2 High-Speed Steel Modified with Titanium diboride

The precipitation of the secondary carbides in high-speed steel of AISI M2 type modified with titanium diboride has been investigated for both the cast and the heat-treated states. The primary focus was on the effect of austenitizing temperatures on the secondary carbide precipitation during tempering. Some differences in origin of the secondary carbides, as well as in their shape and size distribution, were found in the tempered microstructure for the different austenitizing temperatures. After austenitization at 1180 °C and triple tempering at 560 °C, the secondary carbide particles of a spherical shape up to 200 nm in size were identified by selected area electron diffraction as M₂₃C₆. After austenitization at 1220 °C, two types of the secondary carbides were found in the tempered microstructure, M₂₃C₆ with a size up to 200 nm and M₆C with a size up to 400 nm. In both the cases, the carbide particles were slightly angular. After austenitization at 1260 °C, only M₆C secondary carbides were revealed in the tempered microstructure, which occurred as the angular particles up to 350 nm in size. In addition, considerably finer M₂₃C₆ carbide particles with a size of 10-40 nm were found to precipitate in the tempered microstructure.     

Temperature-Dependent Effects of FeS<Subscript>2</Subscript> Thin Film Synthesized by Thermochemical Spraying: An Optical and Physicochemical Investigation

FeS₂ pyrite films are used in a variety of applications including solar cells and, the potential scope for their utilization is increasing as their synthetic methods become more economical while maintaining or enhancing their high light absorption coefficients. The glass substrate temperature dependence on the formation of FeS₂ pyrite films was investigated with respect to their optical and physicochemical properties. During the thermochemical spraying process the temperature was varied in the range of 190-290 °C. FeS₂ nanocrystalline (40-70 nm) films, formed as a result of atmospheric spraying with glass substrate temperatures above 260 °C, were observed by SEM. Opto-electronic studies revealed that the nanocrystalline films had a direct band gap (1.3-1.6 eV) with a high light absorption coefficient (α > 7 × 10⁴ cm^?1 for λ < 1800 nm). Thus, this study offers an alternative to complicated methods for thin-film formation through spaying technology, for the synthesis of high-quality FeS₂ pyrite films with potential application as high light-absorbing solar energy absorbers.     

Comparison of ZrB<Subscript>2</Subscript>-MoSi<Subscript>2</Subscript> Composite Coatings Fabricated by Atmospheric and Vacuum Plasma Spray Processes

In this work, ZrB₂-20 vol.% MoSi₂ (denoted as ZM) composite coatings were fabricated by atmospheric plasma spray (APS) and vacuum plasma spray (VPS) techniques, respectively. Phase composition and microstructure of the composite coatings were characterized. Their oxidation behaviors and microstructure changes at 1500 °C were comparatively investigated. The results showed that VPS-ZM coating was composed of hexagonal ZrB₂, tetragonal and hexagonal MoSi₂, while certain amount of ZrO₂ existed in APS-ZM coating. The oxide content, surface roughness and porosity of VPS-ZM coating were apparently lower than those of APS-ZM coating. The mass gain of APS-ZM coating was maximum at the beginning (1500 °C, 0 h) and then decreased with the oxidation time extending, while the mass of VPS-ZM coating gradually increased with increasing the oxidation time. The possible reasons for the different oxidation behaviors of the two kinds of coatings were analyzed.     

Dependence of Al<Subscript>2</Subscript>O<Subscript>3</Subscript> coating thickness and annealing conditions on microstructural and electrochemical properties of LiCoO<Subscript>2</Subscript> film

We studied the dependence of Al₂O₃ coating thickness and annealing conditions on the surface morphology and electrochemical properties of Al₂O₃ coated LiCoO₂ films. The optimum coating thickness allowing for the highest capacity retention was about 24 nm. A sample consisting of Al₂O₃ coated on annealed LiCoO₂ film with additional annealing at 400 °C had a uniform coating layer between the coating materials and cathode films. This sample showed the best capacity retention of ∼91 % with a charge-cut off of 4.5 V after 30 cycles, while the bare cathode film showed a capacity retention of ∼32 % under the same conditions. The formation of second phases such as Co-Al-O was observed in the coating films by X-ray photoelectron spectroscopy (XPS). The Co-Al-O containing samples showed a higher initial capacity because of their smaller grain size, but less capacity retention than the Al₂O₃ containing samples.     

Ferroelectric properties of dysprosium-doped Bi4Ti3O12 thin films crystallized in various atmospheres

Dysprosium-doped Bi4Ti3O12 （Bi3.4Dy0.6Ti3O12, BDT） ferroelectric thin films were deposited on Pt（111）/Ti/SiO2/Si（111） substrates by chemical solution deposition （CSD） and crystallized in nitrogen, air and oxygen atmospheres, respectively. X-ray diffraction （XRD） and scanning electron microscopy （SEM） were used to identify the crystal structure, the surface and cross-section morphology of the deposited ferroelectric films. The results show that the crystallization atmosphere has significant effect on determining the crystallization and ferroelectric properties of the BDT films. The film crystallized in nitrogen at a relatively low temperature of 650 ℃, exhibits excellent crystallinity and ferroelectricity with a remanent polarization of 2Pr = 24.9 ℃/cm^2 and a coercive field of 144.5 kV/cm. While the films annealed in air and oxygen at 650 ℃ do not show good crystallinity and ferroelectricity until they are annealed at 700 ℃. The structure evolution and ferroelectric properties of BDT thin films annealed under different temperatures （600-750 ℃） were also investigated. The crystallinity of the BDT films is improved and the average grain size increases when the annealing temperature increases from 600 ℃ to 750 ℃ at an interval of 50 ℃. However, the polarization of the films is not monotonous function of the annealing temperature.     

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.     

Corrosion behaviour of polycrystalline Nb<Subscript>2</Subscript>O<Subscript>5</Subscript> thin films and its size effects

This study examines the effect of film thickness ranging from 230 to 404 nm on the corrosion resistance of Nb₂O₅ thin films grown by chemical solution deposition. The films were characterized to obtain the relationships between the deposition parameters and the most relevant physical properties (structural, surface morphology and corrosion resistance). From X-ray diffraction and XPS analyses we can conclude that the films were stoichiometric Nb₂O₅ and crystalline. The internal strain and morphology of the film changes as the number of layers increases indicating a thickness dependent grain size. The surface roughness, corrosion resistance were also affected by the film thickness. Electrochemical impedance spectroscopy (EIS) shows that the thicker film have higher passive and charge transfer resistance than the control samples. These results coating layer of Nb₂O₅ improves the corrosion resistance on an API 5L X80 steel alloy due to the formation of a film on the surface.