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The characteristics of electrophoretic deposition (EPD) of positively charged particles onto a cathode were investigated using aqueous alumina and zirconia suspensions. The deposition was performed using several kinds of metal substrates at different current densities. For most substrate materials, a large number of macropores appeared in the deposit, and their size increased with the current density due to gas bubble formation. However, no macropores were formed in the deposit on a palladium substrate, regardless of the current density. The green density and sintering properties of the EPD deposits on a palladium substrate from aqueous suspensions were the same as from slip casting. Bubble-free zirconia/alumina laminate composites were also fabricated by EPD from aqueous suspensions.
Hydrogenated amorphous carbon thin films were prepared by using organic hydrocarbon source, xylene (C8H10), in a plasma enhanced chemical vapor deposition-(PECVD) system. In contrast to a single broad PL peak from methane (CH4)-based hydrogenated amorphous carbon films, a new PL feature was observed from xylene-based a–C:H films in the blue-green light region. It was found that the aromatic-structures were enhanced in xylene-based a–C:H films deposited at high radio frequency power, which may result in the existence of luminescence centers in the carbon films and induce the appearance of a new PL peak.
The M-phase solid solutions Li1+x−yNb1−x−3yTix+4yO3) (0.1 ≤ x ≤ 0.3, 0 ≤ y ≤ 0.175) in the Li2O–Nb2O5–TiO2 system have promising microwave dielectric properties. However, these compounds can contain small quantities of ferroelectric impurities that affect the polarization response of the material. Due to their low concentration and their chemical similarity to the host material, the impurities cannot be detected by x-ray diffraction or local elemental analysis. Scanning surface potential microscopy and piezoresponse imaging were used to analyze phase compositions in this system. Piezoresponse imaging demonstrated the presence of thin (<200–300 nm) ferroelectric layers on the grain boundaries oriented along the c-axis of the M-phase. Differences between the surface potential and the piezoresponse of ferroelectric multicomponent systems are discussed.
The possibility of localized doping by Er3+ diffusion at moderate (less than 500 °C) temperature was for the first time demonstrated for sapphire single crystal wafers. The doping was achieved by immersing the substrate wafers into reaction melt containing small amounts of erbium salt. The crucial point of the presented technology was a crystallographic orientation of the used wafers. The most suitable orientation of the cuts was the “X-cut” with orientation (11–20). The strong anisotropy of the moderate temperature Er3+ doping into lithium niobate and sapphire was explained on the basis of the crystal structure of particular cuts.
It is shown that to analyze the load versus displacement data obtained from a nanoindentation experiment on a flat surface, it is incorrect to use the so called “reduced modulus,” which includes the elastic properties of both the indenter and the test solid. It is suggested that, until correct analytical solutions become available, the indenter should always be of a much stiffer material than the test solid and it should be approximated to a rigid indenter in the analysis. Furthermore, when the indenter and the test surface are of comparable elastic moduli, the measured indenter displacement is the distance of mutual approach of the two contacting bodies rather than the penetration of the indenter below the original surface of the test solid.
Nanocrystalline Ag–Fe–Ni powders were produced by a reduction of the aqueous metal ion solutions with sodium borohydride and then converted to fine-grained silver–Invar alloys that offer attractive thermal, electrical, and mechanical properties. The samples were characterized by x-ray diffraction, scanning electron microscopy, wavelength dispersive x-ray spectrometry, thermomechanical analysis, microhardness measurements, and electrical conductivity measurements; thermal conductivity was estimated using the Wiedemann–Franz law. Sintering of a specimen with a nominal composition of 60 wt% Ag–25.6 wt% Fe–14.4 wt.% Ni led to the formation of a two-phase silver–Invar alloy with a grain size of approximately 2 μm, a hardness of 133 HK200g, coefficient of thermal expansion of 12.44 × 10−6 / °C, and electrical conductivity of 2.13 × 105 (Ω cm) −1.
On the basis of the first principle interatomic potentials, the site preference of various alloying elements in Fe3Al were evaluated for Ti, Si, Ni, Mn, Mo, and Cr, respectively. The calculated results of the substitutional distribution were in good agreement with the experimental results. Moreover, the calculated results showed that H atoms in Fe3Al prefer to occupy the Fe-type octahedral interstice on the surface, which resulted in concentration of H atoms on the surface. Cr addition decreased the absorbability of Fe3Al-based alloys for H atoms and the force to drive H atoms segregating to surface. The concentration of H atoms on the surface can be decreased by Cr addition.
A ferromagnetic film composed of carbon matrix and dispersed fine iron particles was prepared by heating a polyimide film containing iron complex at temperatures up to 1000 °C. The particles were formed and distributed homogeneously on the film surfaces by heat treatments at 600 °C and above, and inside the films at 700 °C and above. The particles were α–Fe, γ–Fe (or austenite), and Fe3C with fractions of about 7:2:1 in the films heated at 800 °C and above. The mean crystallite sizes of α–Fe and γ–Fe (or austenite) particles were evaluated to be 19 and 15 nm in the film heated at 800 °C, and 32 and 30 nm at 1000 °C, respectively. The films heated at 600 °C and below were superparamagnetic, while those at 700 °C and above were ferromagnetic, but both components existed in all films. The iron particles promoted the growth of carbon crystallites in the films; i.e., the interlayer spacing was about 0.341–0.343 nm and mean crystallite size 4.0–6.5 nm for the films heated in the range of 700 to 1000 °C. Pores were observed on the surfaces and cross sections of the carbonized films, and they seemed to be loopholes of the clusters. Iron oxides were scarcely formed in the films, even after being kept for a long duration at room temperature in atmosphere.
Microscopic effects of self-radiation damage in 244Cm-doped LuPO4 crystals were examined with transmission electron microscopy. These LuPO4 crystals had been doped with 1 wt% 244Cm and exposed to a radiation dose as high as 5 × 1016 α-decay events/mg over 18 years. The microscopic analysis revealed dense arrays of individual defect clusters and numerous bubbles. Whereas, the defect clusters may be interpreted as residuals of alpha-recoil tracks, the bubbles likely resulted from the α-particles generated during the decay events. The bubbles were found to coalesce under electron beam irradiation. Despite the high accumulated dose over the 18 years, the samples exhibited sharp diffraction patterns and periodic lattice spacings. This finding indicated that the samples remained largely crystalline and that the radiation-induced lattice damage was recovered at a rate comparable to that of damage production. This high recoverability is discussed with respect of various annealing processes that may have occurred in the samples.
A ceramic ink was prepared, characterised, and subjected to continuous ink-jet printing. The optimum modulation frequency for printing was estimated. The surface free energies of several substrates were determined and different patterns of the ink droplets were printed on these. Phenomena occurring during the process were investigated. The drop-by-drop resolution and ink spreading were found to be dependent on the dispersive/total surface free energy ratio of the substrates. Ink drying was accompanied by powder migration in the droplets deposited on substrates with a surface free energy lower than the surface tension of the ink. Printing of multiple layers was accompanied by the appearance of ridges, splattering, and non-vertical walls. The causes of these phenomena are discussed in this paper.
The modified edge lift-off test (MELT) has gained enough acceptance in the community for evaluating interfacial adhesion that there is now commercial equipment for automating the test. However, there are several experimental and mechanics assumptions of the test that may provide unexpected outcomes. Experimental data suggested that for crack lengths greater than 5% of the film thickness the energy release rate was independent of crack length, contradicting the rule of thumb suggesting that the crack length should be greater than 10–20 times the film thickness to obtain a steady-state energy release rate in the edge crack problem. Finite element simulations not only corroborated the experimental observation but seemed to indicate that the crack length required for steady-state conditions was a function of the relative Young's moduli for the film and substrate. It was also shown via an analytical model that plate bending (commonly neglected) can significantly affect the energy release rate in the MELT and lead to incorrect conclusions regarding the reliability of an interface.
Cu(In,Ga)Se2(CIGS) thin films were prepared at substrate temperatures of 350 to 500 °C. The (In,Ga)2Se2 precursor layers were deposited on Mo coated soda-lime glass and then exposed to Cu and Se fluxes to form CIGS films. The surface composition was probed by a real-time composition monitoring method. The CIGS films were characterized by x-ray diffraction, energy dispersive x-ray spectroscopy, secondary ion mass spectroscopy, and atomic force microscopy. The transient formation of a Cu–Se phase with a high thermal emissivity was observed during the deposition of Cu and Se at a substrate temperature of 350 °C. Faster diffusion of In than Ga from the (In,Ga)2Se3 precursor to the newly formed CIGS layer was observed. A growth model for CIGS films during the deposition of Cu and Se onto (In,Ga)2Se3 precursor is proposed. A solar cell using a CIGS film prepared at about 350 °C showed an efficiency of 12.4%.
The joining characteristics of oxidized SiC particles with Al–Mg alloy during reaction infiltration processing for fabrication of the composite were studied. From the measurement of weight changes due to the transformation from SiC into SiO2, it became clear that the thickness of SiO2 layer which was formed at the surface of SiC particles increased parabolically with holding time at the given exposing temperatures. The degree of oxidation of the preform made by SiC particles can be controlled by the application of the present oxidation data. The microstructure observed by field emission scanning electron microscopy showed network skeleton via necklike oxidized-joining among the SiC particles and the compressive strength of the perform increased with oxidation temperature. Furthermore, the microstructure of the composite which was fabricated by Al–2 wt% Mg alloy via reaction infiltration processing was examined and the formation of spinel was observed to join the matrix with the particles like a bridge, which is suitable to make the complicate and strong preforms for the near net-shape composites application in electronic packaging.
Microstructure of (Nd, Eu, Gd)Ba2Cu3O7−δ (NEG-123) samples with (Nd, Eu, Gd)2BaCuO5 (NEG-211) particles were observed by transmission electron microscopy. High-resolution electron microscopy observation demonstrated that the density of microstructural defects was small around the NEG-211 secondary phase particles. Furthermore, the 123/211 interfaces were found to be very clean and sharp. Chemical compositional analysis of the submicron secondary phase particles revealed that these fine particles are not composed of NEG-211 but Eu2BaCuO5 (Eu-211) or Gd2BaCuO5 (Gd-211).
We presented a model for the line-width-dependent grain structure statistics in bamboo interconnects. We then showed, using an electromigration simulation, that grain orientation-dependent interface diffusivities constitute a likely mechanism contributing to the variabilities in lifetimes observed in experiments.
Typical titanium-based perovskite oxides Eu1−xBaxTiO3 (x = 0.6−0.8), Eu1−xKxTiO3 (x = 0.2,0.32), and La0.7 (Na,K)0.3TiO3 were synthesized by high pressure and temperature using RE2O3 (RE = La,Eu), TiO2, alkaline, or alkaline earth carbonates as the starting materials. X-ray diffraction data analysis showed that there was a structural transformation in Eu1−xBaxTiO3 by varying Ba content [i.e., from cubic (x = 0.6,0.7) to tetragonal (x = 0.8)], and that samples Eu1−xKxTiO3 and La0.7(Na,K)0.3TiO3 crystallized in the cubic perovskite structure. 151Eu Mössbauer spectroscopy and electron paramagnetic resonance measurements revealed mixed valence of Eu2+/Eu3+ in samples Eu1−xBaxTiO3 and Eu1−xKxTiO3, while Ti ions were present in pure Ti4+ state. Cubic Eu1−xKxTiO3 was metastable, which decomposed into a mixture of perovskite and pyrochlore phases at high temperatures as accompanied by an oxidation process from Eu2+ to Eu3+. For samples La0.7 (Na,K)0.3TiO3, Ti3+ signals were clearly observed. The reduction mechanisms for Eu ions at A site and Ti ions at B site in the perovskite oxides are discussed in terms of the chemical nature of the framework ions and substitution ions under high pressure and temperature.
The tensile creep behavior of yttrium- and lanthanum-doped alumina (at dopant levels below the solubility limit) was examined. Both compositions (100 ppm yttrium, 100 ppm lanthanum) exhibited a uniform microstructure consisting of fine, equiaxed grains. The creep resistance of both doped aluminas was enhanced, compared with undoped alumina, by about two orders of magnitude, which was almost the same degree of improvement as for materials with higher dopant levels (in excess of the solubility limit). In addition, measured creep rupture curves exhibited predominantly steady-state creep behavior. Our results, therefore, verified that the creep improvement in these rare-earth doped aluminas was primarily a solid-solution effect.
Highly c-axis-oriented (Sr,Ba)Nb2O6 (SBN) films were grown on a seeded MgO(100) substrate via sol-gel method. The substrate was preseeded with epitaxial islands of SBN made by breaking up a continuous film into single-crystal islands by pores. Since the number of epitaxial nuclei was increased at the interface between the film and the substrate, the film on a seeded substrate had better highly orientation than that on unseeded substrate. The film having low Sr content exhibited better epitaxial growth because of the distorted unit-cell network and the change of lattice parameters of SBN thin film. For obtaining excellent optical properties, SBN:75 film was prepared on MgO substrate with SBN:25 composition seed layer. Because of low birefringence of refractive indices in the film having high Sr content, the optical scattering loss by the anisotropy of refractive indices was suppressed.
A method to measure friction during scratching at linearly increasing loads in a commercial atomic force/friction force microscope (AFM/FFM) has been developed. The normal load was increased in small increments over the required range for the scratch using a software module while the friction signal was measured via a breakout box and data acquisition computer. Topography images of the scratch were obtained in situ with the AFM in tapping mode with minimal loss of damage event information. This technique was employed to study the scratch resistance of hard amorphous carbon coatings of thicknesses ranging from 20 nm down to 3.5 nm deposited by different commercially available deposition techniques on a silicon substrate.
Employing the n-body potentials of the Ni–Zr and Ni–Ti systems, we performed molecular dynamics simulation to study the relative stability of the terminal solid solutions versus the corresponding amorphous states as a function of solute concentrations. The terminal solid solutions transformed into amorphous states spontaneously when the solute concentrations were beyond the maximum allowable values; i.e., the critical solubilities were determined to be 14 at.% Zr in Ni and 25 at.% Ni in Zr for Ni–Zr system and 38 at.% Ti in Ni and 15 at.% Ni in Ti for the Ni–Ti system. The physical implication of the critical concentrations, as well as their correlation with the glass-forming abilities of the Ni–Zr and Ni–Ti systems, is discussed.