The tin–silver–copper eutectic is a three-phase eutectic consisting of Ag3Sn plates and Cu6Sn5 rods in a (Sn) matrix. It was thought that the two phases would coarsen independently. Directionally solidified ternary eutectic and binary eutectic samples were isothermally annealed. Coarsening of the Cu6Sn5 rods in the binary and ternary eutectics had activation energies of 73 ± 3 and 82 ± 4 kJmol-1, respectively. This indicates volume copper diffusion is the rate controlling mechanism in both. The Ag3Sn plates break down and then coarsen. The activation energies for the plate breakdown process were 35 ± 3 and 38 ± 3 kJmol-1 for the binary and ternary samples respectively. This indicates that tin diffusion along the Ag3Sn/(Sn) interfaces is the most likely the rate-controlling mechanism. The rate-controlling mechanisms for Cu6Sn5 coarsening and Ag3Sn plate breakdown are the same in the ternary and binary systems, indicating that the phases evolve microstructurally independently of one another in the ternary eutectic.

Hexagonal graphitic BN (h-BN) is interesting as a second phase for high-temperature structural ceramics because it has the same crystal structure as graphite, for which fracture strength and Young’s modulus increase with increased temperature. In this study, high-temperature mechanical properties of Si3N4/BN nanocomposite were evaluated to clarify the effect of fine h-BN particles at elevated temperatures. As a result, we found that high-temperature strength and hardness of the nanocomposite were maintained up to high temperatures; also, its Young’s modulus increased gradually, concomitant with elevated temperatures up to 1400 °C. Finally, these properties were compared with those of monolithic Si3N4 and Si3N4/BN microcomposite.

Many intermetallics, such as Ag3Sn, AuSn4, Cu3Sn, Cu6Sn5 (η and η`), Ni3Sn4, and γ–Cu5Zn8 are present in modern solder interconnects as a result of solder chemistry and/or due to the interfacial reaction between solder and metallization scheme. Coarse-grained, single-phase intermetallics are produced by conventional casting followed by annealing for long time. Ambient temperature isotropic elastic moduli (bulk, Young’s, shear, and Poisson’s ratio) and selected plastic properties (hardness and indentation fracture toughness) of these intermetallics are presented. The isotropic elastic moduli of these intermetallics are determined by the pulse-echo technique. The measured bulk, Young’s and shear moduli lie in the range of 6.3 to 11.4 × 1010 N/m2, 7.1 to 12.3 × 1010 N/m2 and 2.7 to 4.5 × 1010 N/m2, respectively. The hardness and fracture toughness are determined by an indentation method. The loads used for indentation experiments were: 100–10,000 g for Ag3Sn and γ–Cu5Zn8, 10–50 g for AuSn4, 200–1000 g for Cu3Sn, 50–100 g for Cu6Sn5, and 100–200 g for Ni3Sn4. The measured Vickers hardness lies in the range of 50 to 470 Kg/mm2, and the measured indentation fracture toughness lies in the range of 2.5 to 5.7 MPa m1/2. Due to coarse grain size of the specimens, the indentation cracks were contained within one grain. In Cu3Sn, Cu6Sn5 (η and η`) and Ni3Sn4 intermetallics, the indentation cracks were found to be nearly straight and run along the indent diagonal. However, the cracks in AuSn4 showed significant zig-zag and branching phenomena, and they seemed to propagate along particular cleavage plane(s). The presence of slip bands are also observed in AuSn4, Ag3Sn, Cu3Sn, γ-Cu5Zn8, and Ni3Sn4. In the case of Ag3Sn and γ–Cu5Zn8, indentation cracks cannot be induced by applying loads up to 10 kg. Rather, extensive plastic deformation occurs resulting in the formation of a large number of shear/kink bands, and possibly twins, that spread across several grains. At a load of 5000 g or higher, Ag3Sn exhibits grain boundary decohesion near the indents. Among the intermetallics studied, Ag3Sn is shown to be the most ductile.

Al2O3-dispersed Yb2O3-stabilized cubic-ZrO2 (YbSZ) composites are fabricated by pressureless sintering of composite powders to obtain fine and homogeneous microstructures by the solution chemistry route. Al2O3 particles are deposited on ZrO2 powders by the precipitation of aluminum nitrate followed by calcination in air. The sinterability of the composites was affected by the calcination temperature. Microstructures of the sintered bodies are dependent on the Al2O3 content. For the5 vol% Al2O3-dispersed composite, fine Al2O3 particles were mainly located insidethe grains of zirconia, whereas relatively large Al2O3 particles almost dispersed at the grain boundaries when the Al2O3 content was increased. The grain growth of YbSZ was suppressed by the Al2O3 addition, and the refinement of the matrix grain improved the fracture strength of YbSZ. The YbSZ and YbSZ/Al2O3 composites exhibited almost similar ionic conductivity at high temperatures of around 1000 °C.

The mechanical properties of monolayer and multilayer structures of several symmetrically substituted alkoxy copper phthalocyanine, CuPc(OR)8, Langmuir–Blodgett (LB) films were evaluated. One-dimensional compliance of the monolayers was determined from the slopes of the surface pressure–area isotherms. Multilayers were examined using a SPM and a commercial nanoindentation system. The nanomechanical studies show a distinct relationship between the position and length of alkoxy substituents on the Pc macrocycle and the LB film elasticity and hardness. The phthalocyanine complexes with peripheral octabutoxy and octaoctyloxy substituents form stiff LB monolayers and multilayers. The nonperipheral alkoxy derivetized CuPc films were less stiff. For monolayer films, it appears that the extent of π-π interaction determines the strength of the film. In multilayers, significant additional stability can be imparted through interdigitation of long paraffinic chains which play a significant role in determining the interlayer structure of the LB layers.

Microstructured biomaterials such as mollusk shells receive much attention at present, due to the promise that advanced materials can be designed and synthesized with biomimetic techniques that take advantage of self-assembly and aqueous, ambient processing conditions. A satisfactory understanding of this process requires characterization of the microstructure not only in the mature biomaterial, but at the growth fronts where the control over crystal morphology and orientation is enacted. In this paper, we present synchrotron microbeam x-ray diffraction (XRD) and electron microscopy observations near the nacre–prismatic interface of red abalone shell. The relative orientations of calcite and aragonite grains exhibit some differences from the idealizations reported previously. Long calcite grains impinge the nacre–prismatic boundary at 45° angles, suggestive of nucleation on (104) planes followed by growth along the c axis. In the region within 100 μm of the boundary, calcite and aragonite crystals lose their bulk orientational order, but we found no evidence for qualitative changes in long-range order such as ideal powder texture or an amorphous structure factor. XRD rocking curves determined the mosaic of calcite crystals in the prismatic region to be no broader than the 0.3° resolution limit of the beamline’s capillary optics, comparable to what can be measured on geological calcite single crystals.

Transmission electron microscopy and x-ray diffraction were used to study SrTiO3 films grown on platinized (0001) Al2O3 substrates. The Pt films were epitaxial with an orientation relationship described by (111)Pt‖(0001)Al2O3 and [110]Pt‖[10¯10]Al2O3. SrTiO3 films with two different Sr to Ti ratios, 1.02 and 1.4, were deposited by radio-frequency magnetron sputtering. In the film with a large amount of Sr excess, the grain sizes were smaller and a high density of planar defects was observed. The films were predominantly (111) textured, but a weaker (110) texture component was also found, independent of stoichiometry. While the (111) texture could be explained with the excellent lattice match with (111) Pt, the (110) textured grains had a large mismatch with the Pt electrode. We propose that the presence of the (110) oriented grains is due to nucleation at Pt surface defects. Planar defects in the films with a large amount of Sr excess served to accommodate the nonstoichiometry. Comparison with homoepitaxial SrTiO3 films showed that the density of planar defects in the SrTiO3 films on (111)Pt/Al2O3 is insufficient to accommodate all the excess Sr. The influence of the film microstructure on the dielectric properties is also discussed.

Highly crystalline-textured pure dense alumina ceramics were fabricated from spherical alumina powder without any seed particles and sintering additives by electrophoretic deposition (EPD) in a strong magnetic field of 10 T. The crystalline texture was confirmed by x-ray diffraction (XRD) for alumina ceramics deposited at 10 T followed by sintering at 1873 K. The angle between the directions of the magnetic and electric fields (φB-E) was altered to control the dominant crystal faces of the α-alumina monoliths. The average orientation angles estimated from the XRD diagram of the samples prepared at φB-E = 0°, 45°, and 90° were 16.52°, 45.15°, and 84.90°, respectively. Alumina/alumina laminar composites with different crystalline-oriented layers were also fabricated by alternately changing the φB-E layer by layer during EPD in a 10 T magnetic field. It was demonstrated that by using this technique, it is possible to control the crystalline orientation by changing the angle of E versus B during the EPD.

Solid solution Pb1-xBaxTiO3, with particular emphasis on Pb0.5Ba0.5TiO3, was prepared using a sol-gel process incorporating lead acetate trihydrate, barium acetate, and titanium isopropoxide as precursors, acetylacetone (2,4 pentanedione) as a chelating agent, and ethylene glycol as a solvent. The synthesis procedure was optimized by systematically varying acetylacetone: Ti and H2O:Ti molar ratios and calcination temperature. The resulting effects on sol and powder properties were studied using thermogravimetric analysis/differential scanning calorimetry, Fourier transform infrared spectroscopy, Brunauer-Emmett-Teller analysis, and x-ray diffraction (XRD). Crystallization of the perovskite structure occurred at a temperature as low as 450 °C. Thin films were prepared by spin coating on (100) MgO. Pyrolysis temperature and heating rate were varied, and the resultant film properties investigated using field-emission scanning electron microscopy, atomic force microscopy, and XRD. Under optimized conditions, highly oriented films were obtained at a crystallization temperature of 600 °C.

Nanocrystalline boehmite obtained by limited hydrolysis of aluminum tri-sec-butoxide or aluminum chloride was aged under different conditions before being calcined above the dehydroxylation temperature. When aging was carried out under hydrothermal conditions, the condensation of the structural units obeyed a first-order kinetic law with apparent activation energy of 12.2 kcal/mol. Under dehydroxylation conditions, the boehmite fragmentation is accounted for by a simple power law that links its volume to that of the resulting γ-alumina. The main variable is the volatile compounds content (water for instance) in the fresh sample. In terms of texture, a better organization of the initial nanoparticles in the boehmite means a lower surface area and larger pore diameter in the corresponding γ-alumina.

Nano-grained phosphors of Eu3+-doped MgGa2O4 crystallites were prepared by sol-gel technique. The characterization and optical properties of luminescent MgGa2O4:Eu3+ powders have been investigated. The dried sol-gel powders were calcined in air at different temperature from 600 to 1000 °C for 5 h. The x-ray diffraction profiles showed that the MgGa2O4:Eu3+ powders began to crystallize around 600 °C and formed stable MgGa2O4 phase in the temperature range of 600–900 °C. The transmission electron microscopy morphology observations revealed that the fired powders exhibit small grain size less than 20 nm. In the PL studies, under ultraviolet (394 nm) excitation, the calcined powders emitted bright red luminescence (615 nm, 5D0→7F2), and the powders fired at 900 °C were found to have the maximum photoluminescence intensity. The quenching concentration of Eu3+ in MgGa2O4 crystallites was also indicated to be about 5∼6 mol%.

Thin films of mixed manganese (mainly 4+) and vanadium (5+) oxides deposited electrochemically on a platinum substrate have been heat-treated under vacuum at various temperatures between 25 and 400 °C. Electron spin resonance and x-ray photoelectron spectroscopy revealed that the reductive formation of Mn2+ occurs at 300 °C only in the presence of vanadium within the film. This phenomenon can be regarded as a result of electron transfer from V4+ ions generated thermally to neighboring Mn sites. Voltammetric response of the heat-treated Mn/V oxide film in borate solution was enhanced with increasing the number of potential cycles, and the steady-state current was much larger than that of pure manganese oxide. Vanadate ions were diffused from the film to maintain the charge balance during the repetition cycles. The resultant porous structure can allow easier mass transport of protons to electrically conductive Mn oxide surface, offering the improved charge–discharge performance of the electrode.

The electrical conduction mechanisms of approximately 8-nm-thick Ta2O5 films grown by metalorganic chemical vapor deposition were investigated by measuring the current density–voltage characteristics at various temperatures. The Ta2O5 films were grown in two steps with or without intermittent annealing at 450 °C under an O3 atmosphere with ultraviolet light radiation (UV-O3 treatment). High-resolution transmission electron microscopy of the films after post-deposition annealing at 750 °C under an O2 atmosphere showed that the intermittent UV-O3 treatment improved the crystallization of the film during post-annealing. Auger electron spectroscopy of the variously treated samples showed that the improvement in crystallization was due to the increase in the oxygen concentration of the Ta2O5 films by the UV-O3 treatment. The Ta2O5 film without the UV-O3 treatment mostly exhibited a Poole–Frenkel conduction behavior with the electron trap level of 0.62 eV from the conduction band edge. The whole layer UV-O3 treated Ta2O5 films also showed a Poole–Frenkel conduction behavior with an almost identical electron trap level and a reduced density. The partially UV-O3 treated Ta2O5 films exhibited a direct tunneling behavior in a relatively low voltage region by the tunneling through the thin (∼3.8 nm) UV-O3 treated surface layer. However, these films showed a Poole–Frenkel conduction behavior in the high-voltage region. In general, the UV-O3 treatment was an efficient method to reduce the leakage current of the high-dielectric Ta2O5 films.

Solid-state recycling for machined chips of pure iron by hot extrusion at 823 K and annealing at 1073–1273 K was carried out. The as-extruded solid recycled specimen without annealing was fractured prior to yielding at room temperature. However, high ductility was recovered by annealing at 1073–1273 K. This is because the oxides at the interface of the machined chips dispersed in grain by annealing. The annealed solid recycled specimens showed higher yield stress than the annealed virgin extruded specimens. Grain refinement for the solid recycled specimens was enhanced by the high dislocation density in the machined chips, resulting in higher strength in the recycled specimens. Thus, the solid-state recycling is a low energy upgrade recycle process.

The structure and mechanical properties of Mg–Zn–Al–Y base cast alloys containing an icosahedral quasicrystal phase (i-phase) as a main strengthening phase were investigated. Mg–8Zn–4Al–xY base bulk alloys containing the i-phase were prepared by casting into a copper mold at moderate cooling rates. The Y addition was effective for decreasing the size of the i-phase and the increasing the homogeneity of its dispersed state. The mechanical properties examined by compression tests at room temperature were much superior to those of a conventional AZ91 Mg alloy. The creep tests at elevated temperatures indicated a promising high temperature creep resistance of the quasicrystal-reinforced Mg–Zn–Al–Y cast alloy. The strengthening mechanism was also discussed.

Amorphous metallic alloys possess high strength characteristics, which are superior to crystalline materials. Here we report an influence of Sc addition on glass-forming ability, glass-transition behavior, supercooled liquid region, and mechanical properties of an Al84Y9Ni5Co2 glassy alloy. This paper also aims to present a promising (Al0.84Y0.09Ni0.05Co0.02)95Sc5 amorphous alloy. This alloy has an ultrahigh tensile fracture strength exceeding 1500 MPa, which surpasses those for all the other Al-based fully crystalline and amorphous alloys reported to date, in addition to high Young’s modulus of 78 GPa. The fracture surface of this new alloy exhibited vein pattern typical for amorphous alloys with good ductility, and multiple shear bandswere observed on the lateral surface. The ultrahigh tensile strength of the (Al0.84Y0.09Ni0.05Co0.02)95Sc5 amorphous alloy results from an increase in the interatomic constraint force by the addition of Sc, an element having highly negative enthalpy of mixing with Al, Ni, and Co and the highest chemical affinity with Al among the alloying elements.

Ag–Pd alloy nanoparticles have been generated from silver and palladium nitrate precursors using a high temperature aerosol method, the liquid flame spray (LFS) process. In the LFS process, a spray aerosol of precursor liquid is introduced into a high-temperature H2–O2 flame. The primary micron-sized spray droplets evaporatein the flame, and the final particulate product is a result of the nucleation of the pure metal vapors shortly after the flame. In the study, three Ag–Pd molar ratios—10:90, 50:50, and 90:10—were used in the precursor. As a result of the synthesis, metalalloy nanoparticles with practically the same concentration ratios, correspondingly, were produced with the method. In the experiments, metal mass flow rates of 0.01–0.8 g/min were covered. The size of the particles was determined to be in the rangeof 10–50 nm by aerosol instrumentation. The particles were spherical and slightly agglomerated. It was concluded that the particle size can be controlled via the total precursor mass flow rate, and the composition can be controlled by the molar ratio of Ag and Pd compounds in the precursor liquid.

We synthesized ultrafine TiO2 nanoparticles by pulsed laser ablation of a titanium target immersed in an aqueous solution of surfactant sodium dodecyl sulfate (SDS) or deionized water. The surfactant concentration dependence of TiO2 nanocrystal formation was systematically investigated by various characterization techniques. The maximum amount of ultrafine anatase nanocrystalline particles (with mean size of 3 nm in diameter) was obtained in an aqueous solution of 0.01 M SDS. A probable formation process was proposed based on the laser-induced reactive quenching and surfactant-mediated growth. The phase transformation and particle growth of as-prepared products were also investigated by heat treatment up to 500 °C. Single-phase anatase nanoparticles with a mean size of 8 nm were obtained by heat treatment of samples prepared in water or in a 0.01 M SDS solution. Particle size did not substantially increase through annealing, probably due to the relatively homogeneous size distribution and crystallinity of as-prepared titania nanoparticles.

The influence of mechanical activation on the characteristics and mechanism of ignition of self-propagating high-temperature synthesis processes of different silicides in the systems Me–Si (Me =Ti, Nb, Mo) was investigated. The results show that mechanical activation does not alter the mechanism involved but influences significantly the ignition characteristics. The influence, however, strongly depends on the stoichiometry of the mixtures. The composition Ti:Si = 1:2 shows the largest influence, with the ignition temperatures decreasing from 1400 °C for unmilled powders to about 600 °C for powders milled for several hours. The compositionsTi:Si = 5:3, Nb:Si = 1:2 show less pronounced decreases, while the compositionMo:Si = 1:2 shows no decrease. These differences are discussed in terms of the role of microstructure in the reaction mechanism and the different response of the systems to contamination, particularly from oxygen. The results suggest that for these systems self-ignition processes during milling cannot be explained only on the basis of the decrease in the ignition temperature.

The effects of heat treatments on strength and electrical conductivity after 100 h in air up to 1500 °C were evaluated on hot-pressed Si3N4–35 vol% MoSi2 composite. The long-term oxidation involves microstructural changes at the material surface and subsurface, such as the formation of oxide scales and of a multilayered microstructure. At T ⩾ 1200 °C, a glassy silicate phase is formed, which embeds cristobalite grains and highly textured Y2Si2O7 crystals. At the same time, MoSi2, assisted by oxygen, reacts with Si3N4 forming Mo5Si3, Si2N2O, and SiO2. The decrease of the room temperature flexural strength reached about 25% in the samples exposed at 1000 °C for 100 h, compared to the as-produced materials. On the contrary, after treatments at higher temperatures, the strength decrease is lower at 1500 °C, the residual strength is 836 ± 62 MPa with a strength decrease of about 8%. The surface oxide scale is an insulator and, consequently, the electrical resistivity of the composite rises from 10-3 to 107–109 Ωcm.