Mechanical and thermal properties of AlN–BN–SiC ceramics

Mechanical and thermal properties were characterized for two AlN:BN:SiC composite ceramics produced from BN with different particle sizes. The ceramics were hot pressed at temperatures from 1950 to 2100 °C to 97% relative density. For both materials, the matrix (90:10 vol% SiC:AlN) had a grain size of 0.4 μm, and the BN grains (10 vol%) were crystallographically aligned. Microhardness values were between 20 and 22 GPa, while fracture toughness values were between 2.5 and 3.1 MPa m^1/2. Other properties were found to be dependent on testing direction. Elastic moduli were between 260 and 300 GPa and strengths were 630 MPa for small particle BN additions. Thermal conductivity was calculated to be between 25 and 37 W/m K at room temperature and 17 and 25 W/m K at 900 °C. The low values compared to traditional SiC ceramics were attributed to AlN–SiC solid solution formation and sub-micron matrix grain sizes.     

Varistor properties and microstructure of ZnO–BaO ceramics

Ceramics in the system ZnO–BaO have been investigated for possible use as varistors. Specimens were prepared by the mixed oxide route, and were sintered at temperatures in the range 1000–1400°C. The electrical properties were determined using d.c. A and impulse techniques. The ZnO–BaO ceramics have a two-phase microstructure comprising a ZnO phase and a Ba-rich grain boundary phase. Due to liquid phase sintering, the average grain sizes for the ZnO–BaO ceramics are large (typically 35–55 m for samples sintered at 1300°C). This results in low breakdown fields, (1000 V cm-1). The maximum non-linearity exponent obtained for ZnO–BaO ceramics (14) is higher than that for binary ZnO–Bi2O3 ceramics. However, the high water solubility of the Ba-rich phase may restrict the use of ZnO–BaO ceramics.     

Microstructure and mechanical properties of nanocrystalline high strength Al–Mg–Si (AA6061) alloy by high energy ball milling and spark plasma sintering

In the present paper, the microstructure and mechanical properties of nanostructured Al–Mg–Si based AA6061 alloy obtained by high energy ball milling and spark plasma sintering were reported. Gas atomized microcrystalline powder of AA6061 alloy was ball milled under wet condition at room temperature to obtain nanocrystalline powder with grain size of 30 nm. The nanocrystalline powder was consolidated to fully dense compacts by spark plasma sintering (SPS) at 500 °C. The grain size after SPS consolidation was found to be 85 nm. The resultant SPS compacts exhibited microhardness of 190–200 HV_100 g, compressive strength of 800 MPa and strain to fracture of 15%.     

Low-temperature fabrication of 0.65 PMN–0.35 PT by a mixed oxide method

Single-phase perovskite 0.65 PMN–0.35 PT was achieved at low temperature by a conventional mixed oxide method. It was prepared by ball-milling a mixture of PbO(orthorhombic), TiO₂, Nb₂O₅ and (MgCO₃)₄Mg(OH)₂·5H₂O instead of MgO and heat treatment at 800 °C for 2 h. The formation was studied by means of DSC, FT-IR, Coupled TG-Mass, XRD, and SEM. It proceeded via formation of PbO(tetragonal) and Pb₂Nb₂O₇(P₂N) intermediates to form perovskite phase. The pure perovskite PMN-PT powder was obtained in particle size of 0.5–0.8 μm, agglomerate-free, and pseudo-cube. The powder calcined at 600 °C was sintered to 97% T.D. at 900–1000 °C for 2 h and showed room temperature dielectric constant of 3200, loss of 1–2%, and specific resistance of 5 × 10¹¹ Ω cm.     

Dielectric and electrostrictive properties of PMNT near MPB

The dielectric constant (ε_r), dielectric loss (tan δ) and strain induced by electric field in lead magnesium niobate–lead titanate (PMN-PT/PMNT) solid solutions in the morphotropic phase boundary (MPB) region at different sintering temperatures have been studied. ε_r and tan δ increase, whereas Curie phase transition range decreases with the increase in sintering temperature. Strain levels in the range of 0.07–0.2% were obtained. A high saturated strain% 0.19, a high d₃₃ coefficient 320 pm/V and a low strain hysteresis% 3.5 in PMNT 68/32 composition sintered at 1200 °C indicate its suitability for actuator applications.     

Effect of environment on fatigue crack growth in ultrafine grain Al–Mg

The fatigue crack growth rates, obtained in high vacuum and in ambient air, of ultrafine grain (UFG) Al–7.5Mg (grain size  250 nm) at various load ratios were compared to those of powder-metallurgy (P/M) Al–7Mg (grain size  2 μm) and ingot-metallurgy (I/M) Al–7Mg (grain size  100 μm). In both vacuum and ambient air, fatigue crack growth rates at all stress ratios decrease with increasing grain size. The fatigue crack growth threshold (ΔK_th) follows the reverse order, increasing with increasing grain size. These trends are interpreted in terms of fracture surface roughness effects that are correlated with grain size. In vacuum, the thresholds of all three materials exhibit no load ratio dependency at load ratios from 0.1 to 0.5. In air, the threshold of UFG Al–7.5Mg exhibits weak load ratio dependency, while P/M and I/M Al–7Mg exhibit modest load ratio dependency. The environmental effect on the fatigue crack growth rates is assessed by determining the difference in crack growth driving force (ΔK) between air and vacuum. It was found that the environmental contribution to the driving force of all three materials is similar, nearly independent of grain size.     

Dynamic recrystallization during high temperature deformation of magnesium

As a consequence of the high critical stresses required for the activation of non-basal slip systems, dynamic recrystallization plays a vital role in the deformation of magnesium, particularly at a deformation temperature of 200 °C, where a transition from brittle to ductile behavior is observed. Uniaxial compression tests were performed on an extruded commercial magnesium alloy AZ31 at different temperatures and strain rates to examine the influence of deformation conditions on the dynamic recrystallization (DRX) behavior and texture evolution. Furthermore, the role of the starting texture in the development of the final DRX grain size was investigated. The recrystallized grain size, measured at large strains (  −1.4) seemed to be more dependent on the deformation conditions than on the starting texture. In contrast to pure magnesium, AZ31 does not undergo grain growth at elevated deformation temperatures, i.e. 400 °C, even at a low strain rate of 10⁻⁴ s⁻¹. Certain deformation conditions gave rise to a desired fully recrystallized microstructure with an average grain size of 18 μm and an almost random crystallographic texture. For samples deformed at 200 °C/10⁻² s⁻¹, optical microscopy revealed DRX inside of deformation twins, which was further investigated by EBSD.     

Optical properties of tungsten disulfide single crystals doped with gold

Single crystals of WS₂ doped with gold have been grown by the chemical vapour transport method using iodine as a transporting agent. X-ray diffraction (XRD) pattern analysis revealed presence of mixed three-layer rhombohedral (3R) and two-layer hexagonal (2H) polytypes for the doped crystals while the undoped one shows only 2H form. Hall measurements indicate that the samples are p-type in nature. The doping effects of the materials are characterized by surface photovoltage (SPV), photoconductivity (PC) and piezoreflectance (PzR) measurements. Room temperature SPV and PC spectra reveal a feature located at 60 meV below the A exciton and has been tentatively assigned to be an impurity level caused by Au dopant. Excitonic transition energies of the A, B, d and C excitons detected in PzR spectra show red shift due to the presence of a small amount of Au and the broadening parameters of the excitonic transition features increase due to impurity scattering. The values of the parameters that describe the electron (exciton)–phonon interaction of excitonic transitions of A–B are about two times larger than that of d–C excitonic pairs. The possible assignments of the different origins of A–B and d–C excitonic pairs have been discussed.     

Structural investigations of sol–gel derived silicate gels using Eu ion-probe luminescence

Undoped and Eu³⁺-doped CaF₂–SiO₂ gels were prepared by the sol–gel method and their optical properties have been studied. The UV–VIS–NIR absorption and photoluminescence spectra have shown the bands typical for the Eu³⁺ ions transitions. When the Eu-doped gel is annealed at temperatures up to 800 °C (i.e. above the CaF₂ crystallisation peak at 460 °C) the photoluminescence spectra intensity increase, the 590 nm (⁵D₀→⁷F₁) and 620 nm (⁵D₀→⁷F₂) luminescence bands become comparable and a structuring of the 620 nm band is observed. The phonon sidebands peaks associated with the ⁵F₀→⁷D₂ transition of the Eu³⁺ ion were observed at around 1000 and 620 cm⁻¹ and have been assigned to the Si–O and Ca–O bonds, respectively. A phonon sideband signal in the range of 300–400 cm⁻¹ was attributed to Ca–F bonds in the precipitated CaF₂ phase. From the optical absorption, photoluminescence and phonon sidebands spectra we have concluded that in the gels annealed at 800 °C, the Eu³⁺ ions are incorporated into the silica network and in the precipitated CaF₂ phase.     

Synthesis, characterization and dielectric properties of nanocrystalline strontium zirconate prepared through a modified reverse micellar route

Nanocrystalline strontium zirconate has been synthesized using a modified reverse micellar route (avoiding Sr-alkoxide). Powder X-ray diffraction studies show the monophasic nature of the powder of SrZrO₃ after heating at 800 °C. The particle size has been obtained from X-ray line broadening studies (62 nm) and transmission electron microscopic studies (72 nm). The average grain size of 85 nm was found to be reasonably stable to sintering till 1000 °C. A dielectric constant of 19.8 is observed for nanocrystalline SrZrO₃ sintered at 1000 °C. Detailed dielectric studies have been carried out with respect to frequency and temperature.     

Investigation of hot ductility in Al-killed boron steels

The influence of boron to nitrogen ratio, strain rate and cooling rate on hot ductility of aluminium-killed, low carbon, boron microalloyed steel was investigated. Hot tensile testing was performed on steel samples reheated in argon to 1300 °C, cooled at rates of 0.3, 1.2 and 3.0 °C s⁻¹ to temperatures in the range 750–1050 °C, and then strained to failure at initial strain rates of 1 × 10⁻⁴ or 1 × 10⁻³ s⁻¹. It was found that the steel with a B:N ratio of 0.19 showed deep hot ductility troughs for all tested conditions; the steel with a B:N ratio of 0.47 showed a deep ductility trough for a high cooling rate of 3.0 °C s⁻¹ and the steel with a near-stoichiometric B:N ratio of 0.75 showed no ductility troughs for the tested conditions. The ductility troughs extended from 900 °C (near the Ae₃ temperature) to 1000 or 1050 °C in the single-phase austenite region. The proposed mechanism of hot ductility improvement with increase in B:N ratio in these steels is that the B removes N from solution, thus reducing the strain-induced precipitation of AlN. Additionally, BN co-precipitates with sulphides, preventing precipitation of fine MnS, CuS and FeS, and forming large, complex precipitates that have no effect on hot ductility.     

Influence of Cu addition on the self-propagating high-temperature synthesis of Ti5Si3 in Cu–Ti–Si system

The self-propagating high-temperature synthesis (SHS) reactions can take place in Cu–Ti–Si systems with Cu additions of 10–50 wt.%, and the products only consist of Ti₅Si₃ and Cu phases, without any transient phase. In Ti–Si system, most of the Ti₅Si₃ grains synthesized exhibit the polygon-shaped coarse appearance with an obviously sintered morphology. When Cu content increases from 10 to 50 wt.%, however, the Ti₅Si₃ exhibits cobblestone-like shape with a relatively smooth surface, and its average size decreases significantly from 15 to 2 μm or less. The formation mechanism of Ti₅Si₃ in Cu–Ti–Si system is characterized by the solution, reaction and precipitation processes. Furthermore, the addition of Cu has a great influence on the volume change between green and reacted preforms. The volume change increases with Cu content increasing from 0 to 20 wt.%, and then decreases with the content further increasing from 20 to 50 wt.%. The addition of Cu to Ti–Si system significantly decreases the onset temperature of the reaction during differential scanning calorimetry process, which is even much lower than the α → β transition temperature of Ti (882 °C), suggesting that the reaction could be greatly facilitated by Cu addition. As a result, the role of Cu serves not only as a diluent but also as a reactant and participates in the self-propagating high-temperature synthesis reaction process.     

Influence of additives on the impact toughness of Al–10.8% Si near-eutectic cast alloys

This article investigates the effects of melt treatment and addition of alloying elements on the impact toughness of as-cast and heat-treated Al–10.8% Si near-eutectic alloys. Increasingly precise impact behaviors are discussed in the context of differentiating between initiation and propagation energies, including the ductility index, which is the ratio of the propagation to initiation energies; total energy as a useful measure is also discussed. Details concerning the evaluation of tensile properties are reported in a separate article [Mohamed AMA, Samuel FH, Samuel AM, Doty HW. Influence of additives on the microstructure and tensile properties of near-eutectic Al–10.8%Si cast alloy. Mater Des, in press]. The concentration of elements in the alloys was changed to the following range: Fe 0.5–1 wt%, Mn 0.5–1 wt%, Cu 2.25–3.25 wt%, and Mg 0.3–0.5 wt%, while the impact toughness upon artificial aging in a temperature range of 155–240 °C for 5 h was also investigated. The results indicate that the morphology of fibrous Si in Sr-modified alloys enhances toughness because of its profound effect on crack initiation and crack propagation resistance. The combined addition of modifier and grain refiner leads to a 33% increase in the impact strength compared to the untreated alloy. In alloys containing high levels of iron, such as the RF2 (1% Fe, 1% Mn) and RF4 (1% Fe, 0.5% Mn) alloys, the addition of iron leads to an increased precipitation of sludge or β-Fe platelets, respectively; these particles also act as crack initiation sites and reduce the impact properties noticeably. In alloys already containing high levels of copper, such as the RC2 (3.25% Cu, 0.3% Mg) and RC5(0.3.25% Cu, 0.5% Mg) alloys, increasing the copper level lowers the impact properties significantly, in view of the fact that the fracture behavior is now predominantly influenced by the Al₂Cu phase rather than by the Si particles. The average crack propagation speed of impact-tested samples shows a good inverse relationship to impact energy. Crack propagation speed can thus provide a qualitative estimation of the impact energy expected for special alloy conditions.     

Silver cofirable Bi1.5Zn0.92Nb1.5O6.92 microwave ceramics containing CuO-based dopants

Bi₂O₃–ZnO–Nb₂O₅ system has emerged as a good low sintering (1050 °C) microwave material because it exhibits high dielectric constant and low temperature coefficient of resonance frequency (τ_f). We have lowered the sintering temperature of Bi_1.5Zn_0.92Nb_1.5O_6.92 (BZN) below 900 °C by using 3 wt.% of CuO-based dopants, such as 0.21BaCO₃–0.79CuO (BC) and 0.81MoO₃–0.19CuO (MC). The doped BZN exhibits high microwave dielectric constant at 2.3 GHz (k  120). The interfacial behavior between BZN and silver was investigated by using X-ray diffractometer, scanning electronic microscope, and electronic probe microanalyzer. The extent of silver migration of MC and BC dopants is reduced at least by one order of magnitude as compared with V₂O₅ dopant when the samples was prepared at 900 °C for 4 h. Thus, CuO-based dopants can replace V₂O₅ to lower the sintering temperature of BZN and to be cofired with silver.     

Nano-crystalline LaFeO3 powders synthesized by the citrate–gel method

A novel sol–gel process was developed for preparing nano-sized, perovskite-type LaFeO₃ powder by the thermal decomposition of the gel-complex of LaFe–(C₆H₈O₇·H₂O). The structural evolution has been systematically investigated by X-ray diffraction (XRD), differential thermal analysis (DTA) and thermogravimetric analysis (TGA). Perovskite powder of  25 nm size could be obtained at a temperature of  600 °C without formation of any secondary phases of La₂O₃ and Fe₂O₃ single oxides and no requirements of high temperature/vacuum/pH control etc. Analysis of the X-ray powder diffraction data showed a decrease in the value of lattice strains with increasing decomposition temperature, whereas the particle size increases with increasing decomposition temperature.     

Forging of Mg–3Al–1Zn–1Ca alloy prepared by high-frequency electromagnetic casting

The 1 wt.%Ca–AZ31 alloy produced by electromagnetic casting (EMC) in presence of electromagnetic stirring (EMS) was extruded and then subjected to the closed-die forging to make a pulley for automobile application. Effective dynamic recrystallization (DRX) took place during the forging process, leading to formation of fully recrystallized grains with the average size of 3–4 μm. High-forging ability and high degree of grain refinement achieved during the forging were attributed to the novel microstructure of the cast composed of small and equiaxed grains with the average size of 50 μm and thin layer (Al, Mg)₂ Ca phase at grain boundaries, which would provide more nucleation sites and a faster rate of recrystallization during deformation by forging as compared to that of the conventionally processed cast composed of large size grains and thick layer (Al, Mg)₂ Ca phase. The forged pulley exhibited the ultimate tensile strength of 273–286 MPa with tensile elongations of 30%. The present result demonstrates a possibility that EMC + EMS techniques can be used in producing magnesium feed stocks with high-forging ability.     

Effect of loading rate on the monotonic tensile behavior and tensile strength of an oxide–oxide ceramic composite at 1200 °C

The influence of loading rate on monotonic tensile behavior and tensile properties of an oxide–oxide ceramic composite was evaluated in laboratory air at 1200 °C. The composite consists of a porous alumina matrix reinforced with woven mullite/alumina (Nextel™720) fibers, has no interface between the fiber and matrix, and relies on the porous matrix for flaw tolerance. Tensile tests conducted at loading rates of 0.0025 and 25 MPa/s revealed a strong effect of rate on the stress–strain behavior as well as on the ultimate tensile strength (UTS), elastic modulus and failure strain. At 0.0025 MPa/s, increase in stress results in non-monotonic change in strain, with the rate of change of strain reversing its sign at stresses 25 MPa/s. Several samples were subjected to additional heat treatments prior to testing in order to determine whether this unusual stress–strain behavior was an artifact of incomplete processing of fibers in the as-received material. The unusual material response in the 0–30 MPa stress range was further investigated in creep tests conducted with the applied stresses ≤26 MPa. Negative creep (i.e. decrease in strain under constant stress) was observed. Porosity measurements indicate that a decrease in matrix porosity and matrix densification may be taking place in the N720/A composite exposed to 1200 °C at stresses <30 MPa for prolonged periods of time.     

Superplastic behavior of a fine-grained ZK60 magnesium alloy processed by high-ratio differential speed rolling

Grain size of the ZK60 alloy was effectively reduced to 12 μm through high-ratio differential speed rolling (HRDSR) for a thickness reduction of 70% in a single pass. Due to the strengthening effects of grain boundaries and particles, the HRDSR processed ZK60 exhibited a high tensile strength of 340 MPa. Low temperature superplasticity was attained at 473–493 K at low strain rates (5 × 10⁻⁴ s⁻¹) and high strain rate superplasticity was attained at 523–553 K at high strain rates (10⁻² s⁻¹). The optimum superplastic temperature was found to be 553 K where a maximum tensile elongation of 1000% was obtained at 1 × 10⁻³ s⁻¹. The deformation behavior of the HRDSR processed ZK60 at elevated temperatures could be depicted by considering contribution of grain boundary sliding and slip creep to total plastic flow. Difference in superplastic deformation behavior between the HRDSR processed and equal channel angular press processed ZK60 alloys was examined and discussed.     

A low-temperature reactive sintering process for the 5Li2O–1Nb2O5–5TiO2 microwave dielectric ceramics

The B₂O₃-doped 5Li₂O–1Nb₂O₅–5TiO₂ composite microwave dielectric ceramics prepared by conventional and low-temperature single-step reactive sintering processes were investigated in the study. Without any calcinations involved, the Nb₂O₅ mixture of Li₂CO₃ and TiO₂ was pressed and sintered directly in the reactive sintering process. More uniform and finer grains could be obtained in the 5Li₂O–1Nb₂O₅–5TiO₂ ceramics by reactive sintering process, which could effectively save energy and manufacturing cost. And relatively good microwave dielectric properties of _r = 41, Q × f = 9885 GHz and τ_f = 43.6 ppm/°C could be obtained for the 1 wt.% B₂O₃-doped ceramics reactively sintered at 900 °C.     

Transformation mismatch plasticity in Pd induced by cyclic hydrogen charging

Transformation mismatch plasticity is achieved in swaged palladium wires by cyclical hydriding–dehydriding. Upon multiple cycles at ambient temperature, a total strain of 40% is accumulated under a constant tensile stress. This value is much higher than the tensile ductility for swaged Pd subjected to monotonic deformation without transformation (<2% for this wire). Strain increments after a single cycle are proportional to the applied stress, in agreement with the Greenwood–Johnson equation for transformation mismatch plasticity. The yield stress of hydrogen-cycled Pd calculated from this equation is 760 MPa, which is much higher than the value of the original wire and about 50% higher than previous values reported for Pd that was hydrogen cycled at 100 °C without an applied stress.