The Pb-free Sn–Ag–Cu–Al solders were investigated for microstructural evolution with respect to Al% and heat treatment. The Al% varies from 0.1% to 0.45% while the contents of Ag are 3.1%–2.53% and of Cu are 0.41%–0.33%. Differential scanning colorimetry (DSC) was applied to identify the melting behavior. A monotectic temperature of 224 °C and a eutectic temperature of 220 °C are deduced from the DSC results. The microstructure was characterized with x-ray diffraction and scanning electron microscopy-energy dispersive spectroscopy. Ag3Sn and the γ2 phase of Al–Cu system are the intermetallic compounds formed in the as-cast solders. Cu6Sn5 formed upon heat treatment for 1000 h at 150 °C in the 0.45 Al-containing solder, while not found in the other solders or other heat treatment conditions. Sn whiskers were detected in a 0.45 Al-containing specimen after aging for 50 h.

Transmission electron microscopy (TEM) was used to study microstructures formed in GaN irradiated with 600-keV O+ ions at room temperature. Three types of defect clusters were identified in the irradiated GaN: (i) basal-plane stacking faults with dimensions ranging from 5 to 30 nm, (ii) pyramidal dislocation loops, and (iii) local regions of highly disordered material. High-resolution TEM imaging clearly revealed that one type of the basal-plane stacking faults corresponded to insertion of one extra Ga–N basal plane in the otherwise perfect GaN lattice. The interpretation of these results indicated that interstitials of both Ga and N preferentially condensed on the basal plane to form a new layer of Ga–N under these irradiation conditions. The formation of these extended defects and their interactions with the point defects produced during irradiation contributed to a dramatic increase in the dynamic recovery of point defects in GaN at room temperature.

The serrated plastic flow of L12 Ni3 (Si,Ti) alloys at intermediate temperature was investigated by tensile tests in terms of the effects of temperature, strain rate, composition, and microstructure. Serrated plastic flow was most strongly observed at 473 K and at a strain rate of 1.6 × 10–4 s–1. Correspondingly, the maximum stress amplitude and the lowest (negative) strain-rate sensitivity were observed at 473 K. Serrated plastic flow took place irrespective of boron doping and was more significant in a fine-grained Ni3 (Si,Ti) alloy. The static aging at 473 K resulted in reduced flow stress. The activation energy for serrated plastic flow was estimated to be about 57 kJ mol–1, suggestive of being smaller than that for lattice diffusion of solutes. The serrated plastic flow behavior of Ni3 (Si,Ti) alloys was compared with that of L12 Co3Ti alloys, and is qualitatively explained on the basis of the dynamics of solutes in the core of a dissociated screw dislocation.

An experimental investigation was undertaken to study low-energy electron exposure effects upon ZnO/K2SiO3 thermal control coating. The specimens were exposed to 10-, 30-, 50-, and 70-keV electrons, respectively. The spectral reflectance of each specimen was measured in situ before and after electron exposures. The solar absorptance was calculated by assuming a Johnson solar spectral irradiance distribution. Electron paramagnetic resonance and photoluminescence measurements were made before and after electron exposures to explain physical changes induced by the electron exposures. All the specimens exhibited a reflectance decrease throughout the visible and the near-infrared regions, and also the induced optical degradation was found to be electron energy dependent, with increased damage for increasing electron energy. It is believed that the optical degradation of ZnO/K2SiO3 thermal control coating, induced by the low-energy electron exposures, is mainly due to the ionization process of the ZnO pigment.

Polyvinylsilane (PVS), derived from vinylsilane by radical polymerization, was partially oxidized in hot carbon tetrachloride solution by flowing air. If the air flow time is adjusted, soft gel films can be formed in a Teflon dish by casting the PVS solution. After the PVS films were peeled from the substrates, they were pyrolyzed at various temperatures. Spectroscopic studies of the pyrolyzed films up to 1273 K suggested that carbosilane (Si–CH2–Si) structures are formed in the films at 473–673 K. The compositions of the amorphous films obtained at 1673 K were approximately SiC1.38O0.21 and SiC1.41O0.51, depending on the crosslinking conditions. The oxygen incorporated in the films was removed in the form of CO and SiO during further heating at 1673–1873 K. The compositions of the films were changed to approximately SiC1.25 and SiC1.26, respectively, at 2073 K. The films obtained at 1273 K did not show degradation during the oxidation at 1273–1673 K while a protective silica layer was formed on their surfaces.

Low thermal conductivity ceramics in the ZrO2–GdO1.5 system have potential in structural (refractories, thermal barrier coatings, thermal protection) and nuclear applications. To that end, the thermal conductivities of hot-pressed xGdO1.5 ·(1 – x)ZrO2 (where x = 0.05, 0.15, 0.31, 0.50, 0.62, 0.75, 0.89, and 1.00) solid solutions were measured, for the first time, as a function of temperature in the range 25 to 700 °C. On the ZrO2-rich side, the thermal conductivity first decreased rapidly with increasing concentration of GdO1.5 and then reached a plateau. On the GdO1.5-rich side, the decrease in the thermal conductivity with increasing concentration of ZrO2 was less pronounced. The thermal conductivity was less sensitive to the composition with increasing temperature. The thermal conductivity of pyrochlore Gd2Zr2O7 (x = 0.5) was higher than that of surrounding compositions at all temperatures. A semiempirical phonon-scattering theory was used to analyze the experimental thermal conductivity data. In the case of pure ZrO2 and GdO1.5, the dependence of the thermal conductivity to the absolute temperature (T) was less than 1/T. Therefore, the minimum thermal conductivity theory was applied, which better described the temperature dependence of the thermal conductivity of pure ZrO2 and GdO1.5. In the case of solid solutions, phonon scattering by cation mass fluctuations and additional scattering by oxygen vacancies on the ZrO2-rich side and by gadolinium vacancies on the GdO1.5-side seemed to account for the composition and temperature dependence of the thermal conductivity.

The crystal structure of microwave dielectric ceramics in the (1 − x)La(Mg0.5Ti0.5)O3 (LMT)–xBaTiO3 (BT) (0 ≤ x ≤ 0.9) system has been refined by Rietveld method using x-ray powder diffraction data. LMT and BT were found to form a solid solution in the whole compositional range. The increase of BaTiO3 content results in the following sequence of structure transformations of those solid solutions: P21/n (a−a−c+, B-site ordered) → Pbnm (a−a−c+) → I4/mcm (a0a0c−) → Pm3m (a0a0a0). These structural changes are related to the disappearance of B-site cation ordering (x > 0.1), in-phase tilting (x > 0.3), and antiphase tilting (x > 0.5), respectively.

The effects of the active and passive protection mechanisms of powder beds on the sintering of Si3N4 were investigated. Shrinkage, density, and coloring behavior of sintered samples were analyzed using different compositions and packing conditions of powder beds based on BN and Si3N4 with different additives. Y2O3 additive in the powder bed influences the weight change and phase formation behavior of the samples, although it has a very low vapor pressure at the sintering temperature. When MgO/Y2O3 was used as sintering additives, the packing density and thickness of the powder bed had a much stronger effect than in the case of Al2O3/Y2O3. For the optimization of the powder bed conditions, the vapor pressure and chemical stability of sintering additives at the sintering temperature has to be considered.

The adsorption/absorption of hydrogen and the adsorption of carbon monoxide by niobium foils, at room temperature, was studied using thermal desorption spectroscopy. Two hydrogen desorption peaks were observed with a maximum at 404 and 471 K. The first hydrogen desorption peak is regarded as hydrogen desorbing from surface sites while the second peak, which represents desorption from surface sites stronger bound to the surface, also has a component—due to its tailing to higher temperatures—of hydrogen diffusing from subsurface sites. Carbon monoxide adsorption was used to determine the number of surface sites, since it does not penetrate below the surface. Two carbon monoxide desorption peaks are observed in these experiments: at 425 and 608 K. The first peak is regarded as the adsorption of molecular carbon monoxide, and the second, as carbon monoxide dissociated on the niobium surface. The crystallographic orientation of the foils was determined by x-ray diffraction and showed a preferential (110) orientation of the untreated foil due to the effect of cold rolling. This preferential orientation decreased after hydrogen/heat treatment, appearing strong also in the (200) and (211) orientations. This change in texture of the foils is mainly due to the effect of heat treatment and not to hydrogen adsorption/desorption cycling. The kinetics of hydrogen and CO desorption is compared with that of Pd and Pd alloys.

We have examined the mechanical behavior of Zr57Ti5Cu20Ni8Al10 bulk metallic glass under uniaxial compression at strain rates from 10−4to 3 × 103 s−1. The failure stress decreases with increasing strain rate, and shear-band formation remains the dominant deformation mechanism. A consideration of basic properties of adiabatic shear bands makes it appear unlikely that shear bands formed under quasi-static loading are adiabatic; in the dynamic case, the time scales of deformation and thermal conduction are similar, indicating that a more sophisticated calculation is required. In the dynamic tests, however, high-speed cinematography reveals evidence that the mechanism of failure involves an adiabatic component.

Advanced analytical transmission electron microscopy has been used to investigate microstructural evolution during pyrolysis in triol-based sol-gel thin films. At pyrolysis temperatures up to 300 °C, the films remained amorphous; however, nanometer-sized precipitates were observed in films heat-treated up to 400 °C for 10 min. Analytical transmission electron microscopy indicated that the precipitates were Pb-rich, as well as deficient in O, Ti, and Zr. Films pyrolyzed up to 500 °C for 10 min were composed of a nanocrystalline pyrochlore phase; however, pores could be observed, situated in the same position as the nanometer-sized precipitates at 400 °C. Face-centered cubic Pb-rich crystallites were also present on the surface of pyrolyzed films but absent in the fully crystallized films annealed at 650 °C. A tentative mechanism is proposed to explain these observations.

After gibbsite was milled for 5 min in a Cr-steel oscillating mill, corundum was obtained by heating the powder for 3 h at 800 °C. We found that iron contamination, produced by the milling process, is essential to attain the transformation at this low temperature and is located at the surface of the gibbsite particles. The knowledge of the oxidation state and location of the contaminant elements, necessary to control the solid-state reactions and/or phase transformations induced by the milling, was realized in this work by a characterization performed by chemical analysis, x-ray photoelectron spectroscopy, Mössbauer spectroscopy, and isoelectric point determination. The iron contamination amounted to about 3% (as Fe2O3) for the sample milled for 60 min. That the iron contamination that occurred mainly on the gibbsite amorphous surface was concluded after a comparison of the isoelectric point determination of the milled samples with that of a mechanical mixture of gibbsite and hematite. X-ray diffraction studies showed that gibbsite looses its crystallinity after the first 5 min of milling.

Powder metallurgy (P/M) methods have expanded in recent years to include net-shape fabrication of W–Cu components. Sintering of W–Cu compacts made from previous powders has led to low density and copper bleedout. This paper presents test results on the consolidation of a new powder containing particles composed of a tungsten-coated copper core. This powder effectively eliminates copper bleedout at sintering thereby making possible the net-shape manufacturing of parts. Sintered articles are characterized by microstructural homogeneity and properties comparable to those of infiltrated W–Cu composites.

Phase-sensitive synchrotron radiation (SR) radiography was combined with x-ray diffraction topography to study structural defects of SiC crystals. The particular bulk SiC crystals examined had a low micropipe density and a hexagonal habitus composed of prismatic, pyramidal, and basal faces well developed. X-ray diffraction topography images of the sliced (0001) wafers, which were formed due to the complex lattice distortions associated with defective boundaries, demonstrated the existence of two-dimensional defective boundaries in the radial direction, normal to the (0001) planes. In particular, those parallel to the 〈1120〉 directions extended rather far from the seed. On the other hand, by phase-sensitive SR radiography the effect of micropipe collection was detected. Micropipes grouped mostly in the vicinities of the defective boundaries but rarely appeared between groups. Some general remarks about possible reasons for the development of such peculiar defect structures were made.

The reliability of coatings that are used in industrial applications critically depends on their mechanical properties. Nanoindentation and scratch testing are well-established techniques to measure some of these properties, namely the elastic modulus and hardness of coatings. In this paper, we investigate the possibility of also assessing the coating fracture toughness and the energy of adhesion between the coating and the substrate using indentation and scratch testing. Various existing and new methods are discussed, and they are illustrated by measurements on particle-filled sol-gel coatings on glass. All methods are based on the occurrence of cracking, and they are therefore only applicable to coating systems that act like brittle materials and exhibit cracking during indentation and scratching. The methods for determining the fracture toughness give comparable results, but the values still differ to within about 50%. The values of the adhesion energy obtained from different measurements are consistent, but it remains uncertain to which extent the obtained values are quantitatively correct. The results show that the methods used are promising, but more research is needed to obtain reliable quantitative results.

Combinatorial chemistry was applied to the optimization of red phosphors used for plasma display panels. Quaternary and ternary combinatorial libraries were developed for (Y, Gd, Lu, Sc)BO3 and (Y, Gd)(BO3 PO4) systems. Our combinatorial chemistry system consists of solution-based combinatorial synthesis and characterization, enabling the swift scanning of luminance and of Commission Internationale de l'Eclairage (CIE) chromaticity under vacuum ultraviolet light excitation. As a consequence of the combinatorial approach, several new candidates were found to show higher luminance than the commercially available red phosphor for plasma display panels.

Materials formed from micro- and nanoscale particles are of interest because they often exhibit novel optical, electrical, magnetic, chemical, or mechanical properties. In this work, a means of constructing particulate materials using DNA strands to selectively attach micro- and nanoparticles to substrates was demonstrated. Unlike previous schemes, the DNA was anchored covalently to the particles and substrates, rather than through protein intermediaries. Highly reproducible selective attachment of 0.11–0.87 mm-diameter particles was achieved, with selective:nonselective binding ratios >20:1. Calculations showed that at most 350 and 4200 DNA strands were involved in the binding of the small and large particles, respectively. Experiments showed that the DNA was bent at an angle, relative to the surfaces of their solid supports.

A symmetrically layered SiC/TiC ceramic with a gradual structure was designed by the finite element method (FEM). After sintering, proper thermal residual stress was introduced into the ceramic due to the coefficients of thermal expansion mismatch between the different layers. After different SiC + C interlayers were inserted into the layers to weaken the interface, the effect of the composition of the SiC + C interlayers between the layers on the residual stress was evaluated. It was found that the weak SiC + C interlayer had little relaxation effect on the residual stress distribution. These ceramics were then fabricated by aqueous tape casting, stacking, and hot-press sintering. An x-ray stress analyzer was used to test the surface stress conditions of the sintered materials. The tested surface stress of the layered SiC/TiC ceramic without interlayer was very close to the FEM calculation. However, there were differences between the tested and calculated results of the layered SiC/TiC ceramics with interlayers; the reason for this was analyzed.

Crystallization and reaction kinetics of a crystallizable K2O–CaO–SrO–BaO–B2O3–SiO2 glass powder with 17–40 vol% titania powder were investigated. The initially amorphous K2O–CaO–SrO–BaO–B2O3–SiO2 glass powder formed cristobalite (SiO2) and pseudowollastonite [(Ca, Ba, Sr)SiO3] during firing. The above crystalline phases were completely replaced by a crystalline phase of titanite [(Ca, Sr, Ba)TiSiO5] when the amount of added titania was greater than a critical value, e.g., 10 vol%, at 99–1100 °C. A chemical reaction taking place at the interface between titania and the glass was attributed to the above observation. The dissolved titania changed the composition of the glass, and the dissolution kinetics was much faster than the formation of cristobalite and pseudowollastonite. Activation energy analysis showed that the crystallization of titanite [(Ca,Sr,Ba)TiSiO5] was controlled by a reaction-limiting kinetics of formation for the Ti–O bond.

Properties of copper films produced using atomic layer deposition (ALD) were characterized. Composition, morphology, and electrical properties of these films grown on glass, as well as Ta, TiN, and TaN on silicon wafers were examined. The resistivity of films thicker than about 60 nm was near bulk value. Films were deposited using a two-step ALD process in which copper(II)-1,1,1,5,5,5,-hexafluoroacetylacetonate hydrate and water vapor were introduced in the first step and a reducing agent was introduced in a subsequent step. Five reducing agents were evaluated, with the best results obtained using isopropanol or formalin. The optimum deposition temperature with isopropanol was about 260 °C, whereas it was about 300 °C with formalin. These films were also investigated as seed layers for electrodeposition of thicker Cu layers for possible interconnect applications. Excellent fills in high aspect ratio trenches were demonstrated.