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.     

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%.     

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.     

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.     

Thin films deposition with ECR planar plasma source

The results of film deposition of pure tungsten as well as intermetallic compound of NdFeB type on various substrates using planar ECR plasma source (with multipole magnetic field) developed in our laboratory are presented. The frequency of 2.45 GHz was generated within the magnetic system by two-slot antenna. The ions of ECR argon plasma are used for target sputtering. The main plasma parameters are density 10¹⁰ cm⁻³, T_e15 eV, ions energy 20 eV, ion current density 3.5 mA/cm² at the ultimate magnetron power. Under sputtering of Nd₈Fe₈₆B₆ target the amorphous films with high adherence and thickness of 5 μm were formed on the substrate. The deposition rate of tungsten films (target biasing 900 V) was 0.59 nm/s. The fine-grained films with high adhesion were obtained. They were tested against heat loads up to 100 J/cm² produced under irradiation of coatings with plasma streams.     

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.     

Near infrared quazi-omnidirectional reflector in chalcogenide glasses

The quazi-omnidirectional reflector was designed as a planar quarter wave stack consisting of the alternating amorphous chalcogenide Ge₂₅S₇₅ and Sb₄₀Se₆₀ films. Photonic bandgap calculation of the intended reflector predicted 240 nm omnidirectional and 450 nm normal incidence first-order bandgaps centred near 1.55 μm for appropriate values of the index of refraction and thickness of the films. The TEM and HR-TEM images of the prepared 7.5 pairs reflector verified good periodicity, smooth interface and amorphous structure of the chalcogenide films deposited by thermal and flash evaporation, respectively. The optical reflectivity measurements revealed 98.8% normal incidence stopband of the reflector at 1.55 μm. We also report the ellipsometry study of the prepared reflector. The TEM and ellipsometry studies confirmed the thickness variation of prepared individual layers to be ±7 and ±9 nm, respectively, compared to theoretical predictions.     

Luminescence properties of Sr5(PO4)3Cl:Ni nanocrystals

Strontium chloroapatite (Sr₅(PO₄)₃Cl) nanocrystals doped with Ni²⁺ ions were synthesized by a precipitation method. The obtained nanocrystals appeared to be rod-like with diameters of  50 nm and lengths of 150–350 nm by transmission electron microscopy (TEM). The photoluminescence (PL) properties of Ni²⁺ ions in strontium chloroapatite were studied by photoluminescence spectroscopy.     

The influence of Yb doping on the upconversion luminescence of Pr in aluminum oxide based powders prepared by combustion synthesis

The effect of ytterbium (Yb³⁺) doping on the upconversion (UC) emission of praseodymium (Pr³⁺) doped in aluminum oxide based powders prepared by combustion synthesis is reported for near-infrared excitation (λ = 980 nm). Our experimental results show that the crystalline structure and the UC emission changes with the Yb³⁺ concentration. The sample containing only Pr³⁺ (1.0 wt.%) did not show any UC signal and the UC emission profiles of the samples containing Pr³⁺ (1.0 wt.%) and Yb³⁺ (0.5, 2.0 wt.%) are quite different. The sample containing 0.5 wt.% of Yb³⁺ has five emission lines in the visible range associated to Pr³⁺ 4f–4f transitions, ³P₀ → ³H₄ (497 nm), ³P₀ → ³H₅ (525 and 550 nm), ³P₀ → ³H₆ (620 nm) and ³P₀ → ³F₂ (650 nm). We believe that the UC process has its origin in energy transfer from Yb³⁺ ions to Pr³⁺ ions in Pr_0.83Al_11.83O₁₉ phase. The sample containing 2.0 wt.% of Yb³⁺ has only one emission line in the visible range peaked at 507 nm which we believe has its origin in cooperative UC emission due to excited Yb³⁺ pairs in YbAlO₃ phase. The samples containing Yb³⁺ also present UC emission lines in the near-infrared which are assigned to intrinsic lattice defects.     

Visualization of emitting sites on carbon fiber cathode by surface treatment in high-current vacuum discharge process

In this paper, a carbon fiber cathode, having robust, easily shaped, and epoxy-free properties, is constructed by squeeze casting technique that can overcome some disadvantages of conventional methods. Carbon fiber emitters on the cathode surface had a high distribution density, thus ensuring sufficient emission centers or emission uniformity. The fabricated cathode was tested in a diode powered by a 350 kV, 40 Ω, 400 ns high-voltage pulse generator. The turn-on electric field was estimated to be 50 kV/cm, and the field enhancement factor was (1.2–2.0) × 10³. It was found that the electron emission of carbon fiber cathode is initiated from the individual bright spots at a current density of up to 400 A/cm². Most notably, the X-ray images of electron beam on anode foil demonstrate the development of bright spots on the cathode surface. As a whole, this class of cathodes can endure high-current pulsed emission, and has a positive application prospect.     

Preparation of ceria nanoparticles embedded in PMMA using sonochemical technique

Homogeneous distribution of semicrystalline ceria in polymethylmethacrylate has been reported. The ceria has been prepared by sonochemical method, in situ. The as-prepared composite was characterized by XRD, TEM, DSC and TGA methods. An average size of the ceria is found to be  5 nm by XRD and TEM measurements. The photonic band gap has been measured as 3.55 eV, which is in well agreement with the ceria crystals, indicating absence of a quantum size effect.     

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.     

From iron(III) precursor to magnetite and vice versa

The syntheses of nanosize magnetite particles by wet-chemical oxidation of Fe²⁺ have been extensively investigated. In the present investigation the nanosize magnetite particles were synthesised without using the Fe(II) precursor. This was achieved by γ-irradiation of water-in-oil microemulsion containing only the Fe(III) precursor. The corresponding phase transformations were monitored. Microemulsions (pH  12.5) were γ-irradiated at a relatively high dose rate of 22 kGy/h. Upon 1 h of γ-irradiation the XRD pattern of the precipitate showed goethite and unidentified low-intensity peaks. Upon 6 h of γ-irradiation, reductive conditions were achieved and substoichiometric magnetite (Fe_2.71O₄) particles with insignificant amount of goethite particles found in the precipitate. Hydrated electrons , organic radicals and hydrogen gas as radiolytic products were responsible for the reductive dissolution of iron oxide in the microemulsion and the reduction Fe³⁺ → Fe²⁺. Upon 18 h of γ-irradiation the precipitate exhibited dual behaviour, it was a more oxidised product than the precipitate obtained after 6 h of γ-irradiation, but it contained magnetite particles in a more reduced form (Fe_2.93O₄). It was presumed that the reduction and oxidation processes existed as concurrent competitive processes in the microemulsion. After 18 h of γ-irradiation the pH of the medium shifted from the alkaline to the acidic range. The high dose rate of 22 kGy/h was directly responsible for this shift to the acidic range. At a slightly acidic pH a further reduction of Fe³⁺ → Fe²⁺ resulted in the formation of more stoichiometric magnetite particles, whereas the oxidation conditions in the acidic medium permitted the oxidation Fe²⁺ → Fe³⁺. The Fe³⁺ was much less soluble in the acidic medium and it hydrolysed and recrystallised as goethite. The γ-irradiation of the microemulsion for 25 h at a lower dose rate of 16 kGy/h produced pure substoichiometric nanosize magnetite particles of about 25 nm in size and with the stoichiometry of Fe_2.83O₄.     

Survey of the 1997, 1998 and 1999 annual technical reports on patent information activities (part II: I to Z)

The activities of 59 intellectual property offices and organisations worldwide in the field of patent information are summarised for the period 1997–1999. The summary is presented under eight standard headings, as far as relevant, for each country. Activity varies enormously from just a handful of applications through to RU (24K), GB (30K), DE (58K), KR (80K), EP (121K), US (270K utility patents), and Japan (405K); the numbers are continuing to increase significantly in most countries. This part (second of two) covers 35 countries and organisations, with WIPO codes starting I to Z.The author concludes, inter alia, that

(i) the number of patent applications is increasing at such a rate that the granting or registration activities of many IP Offices are unable to keep up;

(ii) the development of electronic filing systems is proceeding apace;

(iii) the IPC, or derivatives such as ECLA, continue to be the primary tools for allocation, classification, and search in all IP Offices, except US and GB;

(iv) automated search systems continue to be developed and are used in tandem with manual search files, commercial and free Internet online databases; and

(v) the use of complex jukebox systems to handle the vast numbers of patent specifications on CD-ROM continues to increase.

Preparation and characterization of ultrafine alumina via sol–gel polymeric route

Ultrafine alumina powder was prepared through resin formation between urea and formaldehyde. Aluminium stearate soap was introduced during resin preparation. Ethylene glycol was used to terminate the thermosetting reaction. Calcination of the product was carried out at 700, 1000, 1100, 1300 and 1400 °C to obtain aluminium oxide.IR and Raman spectroscopic analysis indicated the occupation of Al³⁺ at different sites in the polymer network (CO, NH₂, CO, NH, and CH₂OH).X-ray diffraction of powder calcined at 1000 °C revealed the presence of a mixture of α- and θ-alumina together, while a mixture of α- and β-alumina phases were obtained on calcination at 1400 °C. Transmission electron microscope (TEM) examination of the powder fired at 700 °C showed uniform grains in the form of clusters with average size between 22.02 and 30.5 nm. Clusters are multi-particles as evident from the electron diffraction pattern. Crystallite size of alumina powder calcined at 1000 °C was found to be ≈25.67 nm, while that of powder calcined at1400 °C was ≈30.52 nm. The calculated specific surface area of alumina powder calcined at 1000 °C was 59.17 m² g⁻¹, while that calcined at 1400 °C was 49.77 m² g⁻¹.     

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.     

High specific strength Mg-based bulk metallic glass matrix composite highly ductilized by Ti dispersoid

Mg-based bulk metallic glass matrix composite with hcp-Ti powders was fabricated by casting the mixtures of Mg₆₅Cu₂₅Gd₁₀ molten alloy and pure Ti powders into a copper mold. Ti powder was spherical and less than 150 μm in diameter, and its volume fraction was controlled from 5 to 40%. Thermal stability of the glassy matrix was maintanied even in the coexistence with the Ti powders. However, Ti dispersoid caused a significant improvement on compressive ductility from 0% plastic deformation for the monolithic glass to 41% plastic deformation for the composite with 40 vol.% Ti powders. This is the first success of synthesizing Mg-based alloys with high ultimate strength of 900 MPa level as well as the large plastic deformation of 40%, and suggests a novel guideline to develop Mg-based alloys having high specific strength with high ductility.     

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.     

Environmental sensitivity and mechanical behavior of boron-doped Fe–45at.%Al intermetallic in the temperature range from 77 to 1000 K

The tensile properties and fracture behavior of a coarse-grained (grain size 420 μm) Fe–45at.%Al intermetallic doped with 0.05 at.% boron were examined at ambient temperature in air, argon and vacuum as well as in the 77–1000 K temperature range in liquid nitrogen, dry ice and air. Before testing the alloy was low temperature annealed (vacancy annealed) in order to remove all the retained vacancies. At ambient temperature ductility increases accordingly to decreasing water vapor (moisture) content in each environment. The mixed transgranular cleavage (TGC)+intergranular failure (IGF) mode in vacuum, which is associated with the highest elongation (6%), exhibits around 40% of IGF and the mixed fracture mode in argon, which is associated with the second highest elongation (3.2%), exhibits 15% of IGF. The TGC fracture mode in air is associated with the lowest elongation (1%). Elongation in the cryogenic temperature range from 77 to 213 K is very low being in the range from 0.6 to 2.8%, and is associated with a mixed transgranular+intergranular fracture mode. Elongation increases gradually from 300 to 800 K attaining a ductility peak at 800 K and then decreases rapidly with increasing temperature. At 600–800 K, the yield strength of Fe–45Al–0.05B exhibits anomalous temperature dependence with the yield strength peak at 800 K. The mode of fracture from 300 to 700 K is predominantly TGC and that at the ductility peak is ductile rupture with very deep dimples. At temperatures above 800 K the mode of fracture changes to a typical intergranular creep (fibrous) failure with numerous flat dimples (voids/cavities) at the grain boundary facets, which is associated with a tensile ductility drop. Fine particles (borides) are observed at the grain boundary facets, which assist the development of intergranular creep fracture.     

Superplastic flow in a nanostructured aluminum alloy produced using high-pressure torsion

Samples of a spray-cast Al-7034 alloy were processed by high-pressure torsion (HPT) at temperatures of 293 or 473 K using an imposed pressure of 4 GPa and torsional straining through five revolutions. Processing by HPT produced significant grain refinement with grain sizes of 60 and 85 nm at the edges of the disks for the two processing temperatures. In tensile testing at room temperature, the alloy processed by HPT exhibited higher strength and lower ductility than the unprocessed material. Good superplastic properties were achieved in tensile testing at elevated temperatures with a maximum elongation of 750% for the sample processed at 473 K and tested in tension at 703 K under an initial strain rate of 1.0 × 10⁻² s⁻¹. The measured superplastic elongations are lower than in samples prepared by equal-channel angular pressing because of the use of very thin disks in the HPT processing.