(Na2O,BaO)–Nb2O5–SiO2 and (K2O,SrO)–Nb2O5–SiO2 glass ribbons with varying proportions of alkali and alkaline earth were formed using roller quenching. (Na2O,BaO)–Nb2O5–SiO2 glasses of compositions devitrified to form Ba2NaNb5O15 (in the form of ∼80 nm crystallites in an amorphous matrix) yielded frequency-stable dielectric constants of ∼250 and losses of ∼0.05. Such low losses and frequency stabilities were also observed from (K2O,SrO)–Nb2O5–SiO2 glasses of compositions forming predominantly KSr2Nb5O6 (∼30 nm crystals), yielding dielectric constants of ∼400. Both optimized compositions showed moderate decreases in dielectric constant with increasing temperature.

We have undertaken the exploration of AlxSi1−x material systems to discover new alloys with enhanced mechanical properties. Combinatorial methods were used to systematically control thin film microstructure through variations in composition and growth temperature. Discrete libraries of compositionally graded films have been sputter deposited onto silicon substrates to produce two structural phase regions: amorphous Al–Si and amorphous Si plus crystalline Al. The mechanical properties of the thin films were determined through indentation experiments by analyzing the load–displacement traces based on the Oliver–Pharr method. X-ray diffraction was used to investigate the microstructures and determine the crystallite sizes. In samples with an Al concentration near 55 at.%, the data show that decreasing the Al crystallite size by nearly one half increases the nanocomposite hardness by nearly a factor of two.

The surface properties of some freshly cleaved, or polished, quaternary tellurite glasses (TeO2-ZnO-Na2O-Yb2O3and TeO2-ZnO-Na2O-GeO2) and a proposed ternary fluorotellurite core/clad optical fiber pair (TeO2-N a2O-ZnF2) were investigated by means of x-ray photoelectron spectroscopy and chemical durability. Semiquantitative chemical analysis of the x-ray photoelectron spectroscopy spectra of cleaved tungsten-tellurite and fluorotellurite glasses showed good agreement with the batched at.% values when taking into account the effects of processing (e.g., melt fluorine volatilization), and the samples seemed to exhibit negligible hydrolysis. However, spectra of polished surfaces did not yield useful data because of masking of the glass “signal” from organic contamination at the sample surface. The chemical durability of these glasses were studied; specifically, the glass resistance to the attack and the etchability of various acids (aqueous HF, H2SO4, and HCl), alkali (aqueous NaOH), and water at 15, 21, and 60 °C were obtained by simple mass loss experiments and optical microscopy. Based on the appearance of the glass surfaces after immersion in these solutions, aqueous HF was found to be the most promising etchant, however, infrared spectra showed that significant OH was introduced into the glass. Attack of the fluorotellurite glasses was found to proceed at a higher rate in water at 60 °C compared with room temperature, and at both temperatures was shown to be diffusion controlled, with an Arrhenian activation energy estimated as 57 kJ mol−1.

Microstructure of sintered nanocrystalline SiC is studied by x-ray line profile analysis and transmission electron microscopy. The lattice defect structure and the crystallite size are determined as a function of pressure between 2 and 5.5 GPa for different sintering temperatures in the range from 1400 to 1800 °C. At a constant sintering temperature, the increase of pressure promotes crystallite growth. At 1800 °C when the pressure reaches 8 GPa, the increase of the crystallite size is impeded. The grain growth during sintering is accompanied by a decrease in the population of planar faults and an increase in the density of dislocations. A critical crystallite size above which dislocations are more abundant than planar defects is suggested.

Single phase of Ba1−xZnxGd0.75Tb0.25B9O16 and BaGd0.75−xCexTb0.25B9O16 (0 ≤ x ≤ 0.125) was prepared by the solid-state reaction. Under 254 nm excitation, Zn2+ impaired the emission of Tb3+; Ce3+ sensitized the luminescence of Tb3+ ascribing to the energy transfer of Ce3+ → Tb3+ and/or Ce3+ → Gd3+ → Tb3+ occurring, and the optimum emission was observed at x = 0.05 in BaGd0.75−xCexTb0.25B9O16. Under 147 nm excitation, Zn2+ sensitized the emission of Tb3+ and the optimum emission was obtained at x = 0.075 in Ba1−xZnxGd0.75Tb0.25B9O16, which could be due to the fact that the energy absorption relating to Zn2+ occurred and the absorbed energy was transferred to Tb3+ finally; Ce3+ depressed the luminescence of Tb3+, which could be attributed to the fact that Ce3+ has no absorption in vacuum ultraviolet region and the role of Gd3+ was weakened. Compared with BaGd0.75Tb0.25B9O16 and the commercial phosphor Zn2SiO4:Mn2+, the optimum phosphor Ba0.925Zn0.075Gd0.75Tb0.25B9O16 exhibited about 127% and 51% integrated emission intensity respectively and the shorter decay time of about 2.822 ms under 147 nm excitation.

Spherical indents in NiTi shape memory alloys can have reversible depth change: deeper depth in the martensitic phase at low temperature and shallower depth in the austenitic phase at high temperature. This is the indentation-induced two-way shape memory effect. After polishing the indents, two-way reversible surface protrusions can occur on the shape memory alloy surfaces upon heating and cooling. The height of the surface protrusion is about the same as the depth of the reversible indent. Further polishing reduces the height of the surface protrusion, which disappears completely when the polished depth is about the length of the contact radius. By comparing finite element analysis and experimental data, we show that the depth at which a protrusion disappears is close to the 10% strain boundary. This suggests that slip-plasticity is responsible for the observed indentation-induced two-way shape memory effect.

We present an experimental methodology for locating and studying local failure sites in multilayer electroceramic devices at the submicron-length scale. In particular, the inhomogeneous degradation of multilayer ceramic capacitors is studied using a judicious combination of scanning electron microscopy (SEM), local-probe electrical measurements, focused ion beam (FIB) extraction, and transmission electron microscopy (TEM). Voltage-contrast SEM permits the identification of regions of different electrical potential within degraded multilayer devices. The local impedance from specific regions is measured in situ between a tungsten probe and the internal device electrodes, while impedance spectra are extracted for more detailed analysis. Because implementation occurs in dual-beam FIB/SEM, these locally defective sites can be extracted and thinned to electron transparency for further investigation by TEM. In this study, degraded sites in BaTiO3 multilayer capacitors are found to be associated with local oxygen deficiencies in BaTiO3, as measured by electron energy loss spectroscopy.

In this study, we investigated the role of a minor alloying element in improving the plasticity of amorphous alloys. The plasticity of the amorphous alloys, Cu60−xZr30Ti10Bex, was drastically improved with increasing amount of Be and reached a maximum of 23% at Cu53Zr30Ti10Be7. It was observed that an atomistic-scale phase separation existed within the alloy, which resulted from the large difference in mixing enthalpy between the binary pairs (Be–Cu, Be–Zr). This atomistic-scale phase separation resulted in an open structure in which atomic rearrangements in the form of the creation of free volume and crystallization were facilitated during deformation. Here we discuss the origin of the enhanced plasticity by clarifying the effect of an additional element, whose mixing enthalpies with the major elements are significantly different, on the structural change of the amorphous alloy.

Zr50Cu40Al10, Zr50Cu30Al10Ni10, and Zr50Cu37Al10Pd3 (in at.%) are bulk metallic glasses (BMGs) with partial crystallization that were characterized by x-ray diffraction (XRD). The study of mechanical properties was conducted in compression at room temperature. Four-point-bend fatigue experiments were performed on the zirconium (Zr)-based BMGs in air. Under compressive loading, after the elastic deformation, no obvious plasticity occurred before the final shear fracture. The compression strengths are comparable to those of fully amorphous alloys. However, the fatigue-endurance limits of these BMGs were much lower than those of fully amorphous alloys. These results suggested that the fatigue behavior of a BMG is very sensitive to the microstructure, while the compression strength is not.

The dynamic shear deformation process and the related stacking fault transitions in TiAl have been systematically investigated using both the molecular dynamics and ab initio methods. The details of the dislocation initiation and microstructural evolution are presented, and the concomitant potential energy variation and the radial distribution functions have been analyzed. The results show, interestingly, that some deformation-induced hexagonal close-packed (hcp) structures are metastable, and that a higher velocity field promotes more hcp segments. The phenomena are interpreted based on ab initio calculations of the detailed energy variation at the different fault transition stages, i.e., superlattice intrinsic stacking fault (SISF) → TWIN, SISF → hcp, and hcp → TWIN. The intrinsic factor that governs the deformation process is discussed. The results promote new understanding of the stress-induced interfaces and dislocation behaviors in experimental observations.

The factors governing the transport properties of yttrium-doped barium zirconate (BYZ) have been explored, with the aim of attaining reproducible proton conductivity in well-densified samples. It was found that a small initial particle size (50–100 nm) and high-temperature sintering (1600 °C) in the presence of excess barium were essential. By this procedure, BaZr0.8Y0.2O3−δ with 93% to 99% theoretical density and total (bulk plus grain boundary) conductivity of 7.9 × 10−3 S/cm at 600 °C [as measured by alternating current (ac) impedance spectroscopy under humidified nitrogen] could be reliably prepared. Samples sintered in the absence of excess barium displayed yttria-like precipitates and a bulk conductivity that was reduced by more than 2 orders of magnitude.

Fast degradation rates in the physiological environment constitute the main limitation for magnesium alloys used in biodegradable hard tissue implants. In this work, the corrosion behavior of AZ91 magnesium alloy in simulated body fluids (SBF) was systematically investigated to determine its performance in a physiological environment. The influence of the main constituent phases on the corrosion behavior was studied by in situ visual observation and scanning electron microscopy. Energy dispersive x-ray spectrometry and Fourier transfer infrared spectroscopy revealed that both calcium and magnesium phosphates are present in the corroded products besides magnesium oxide. Electrochemical methods including open circuit potential evolution and electrochemical impedance spectroscopy were used to investigate the mechanism. The corresponding electrode controlled processes and evolution of the corrosion products layer were discussed. The degradation rate after immersion in SBF for seven days was calculated from both the weight loss and hydrogen evolution methods.

P-doped titanium dioxide (TiO2) nanoparticles were synthesized using a sol-gel method. The ethanol solution of Ti(OC2H5)4 was mixed with an aqueous solution of H3PO4 to undergo hydrolysis and polycondensation at 90 °C for 4 h. The resultant solids were centrifugally filtered, dried, and then calcined at different temperatures, followed by chemical and physical characterization. At an atomic ratio of P/Ti = 0.03, the formed P-doped TiO2 can preserve its anatase structure at 900 °C for 3 h, with no formation of other phases. Further increasing the P/Ti atomic ratio in the P-doped TiO2 may stabilize the anatase–TiO2 at even higher temperatures but may lead to the formation of TiP2O7 or (TiO)2P2O7. A test of photocatalysis showed that the P-doped TiO2 nanoparticles, with a P/Ti ratio = 0.03 and after being calcined at temperatures between 400 and 800 °C, can decompose ⩾98 mol.% of the methylene blue (MB) after 30 min of irradiation by 365-nm ultraviolet light, while P25 particles can only decompose 71 mol% of the MB.

A new drying-induced forming (DIF) of ceramics has been developed using high solid-loaded alumina slurries with addition of glycerol, in which the slurry was simply dried in an open mold at the ambient condition. The drying-induced forming approach is facilitated by the high stability of concentrated slurries during drying where glycerol was added to maximize the critical solid loading and play simultaneously as a drying control agent. The drying and rheological behaviors of slurries were examined with respect to the glycerol addition. A slurry of 60 vol% solid loading with 20 wt% glycerol addition was chosen for the drying induced forming test. The green samples exhibited no bending or cracks, and a small degree of shrinkage anisotropy during sintering. The sintered samples showed a high relative density of 99.2% and an average strength of 420 MPa. We demonstrate here a possibility of producing near-net-shaped and bulk ceramic components in a simple scheme by using the drying-induced approach.

Powders of the solid lead-free piezoelectric ceramic solution [Na0.5K0.5NbO3]1−x–[LiTaO3]x, x = 0.06, were produced using a mixed-oxide process. Phase analysis indicated the formation of an orthorhombic solid solution at 800 °C, which coexisted with intermediate binary niobate and tantalate phases. A tetragonal main-phase solid solution was formed at ⩾950 °C, along with minor quantities of a tungsten bronze phase. Addition of 3 wt% excess alkali carbonates to the starting powders allowed the orthorhombic solid solution to be retained to 1100 °C and prevented formation of the secondary tungsten bronze phase. Elemental chemical analysis confirmed changes in alkali oxide composition, consistent with volatilization losses, particularly of potassium and lithium oxides. Phase stability near the reported morphotropic phase boundary is shown to be sensitive to alkali oxide content.

Organic–inorganic hybrid materials were prepared by sol-gel processes starting from tetraethoxysilane (TEOS) and a triethoxysilane-terminated polyethylene–b-poly(ethylene glycol) copolymer (PE–PEG–Si). Curing of the initial reactant solution was carried out under different reaction conditions, and the materials so obtained were investigated by solid-state nuclear magnetic resonance (NMR). In particular, the molecular structure resulting from a conventional oven heating was compared with that obtained by unconventional microwave heating. The results highlighted that the extent of condensation reactions occurring over several hours under conventional heating is very similar to that resulting in 1 min under microwave heating. Additionally, 29Si–magic angle spinning (MAS) spectra showed that even though the overall extent of cross-linking in the inorganic network is only slightly affected by the thermal history of the sample, significantly different distributions of silicon sites can be present. 13C–CP/MAS selective spectra revealed the presence of PE “crystalline” domains within the organic phase, not detectable by differential scanning calorimetry (DSC). Finally, 1H–MAS spectra showed that different hydrogen-bond interactions are present in samples obtained under different curing conditions.

PbTiO3 (PTO) and PbZr1-xTixO3 (PZT) films on a (100) Nb-doped SrTiO3 (NSTO) substrate were fabricated at 160 and 210 °C, respectively, by hydrothermal epitaxy below the Curie temperature, TC. The PTO capacitor had a square hysteresis curve compared to the rounded hysteresis curve of the PZT capacitor. These differing behaviors in the polarization-electric hysteresis curves can be explained by the existence of an interfacial layer formed between the PZT film and the NSTO substrate. The PZT capacitor showed almost no polarization fatigue after 1011 switching cycles. However, the PTO capacitor revealed a slightly different fatigue behavior due to the microvoids that formed as a result of the agglomeration of the island growth mode. However, the fatigue behavior of both capacitors revealed that defects, such as the lead or oxygen vacancies, were suppressed by the hydrothermal epitaxy using a very low fabrication temperature below TC.

Partial and integral enthalpies of mixing of liquid Ag–Cu–Ni–Sn alloys were determined at 1000 °C by a drop calorimetric technique using a Calvet type microcalorimeter. They were obtained by adding Ni to the ternary Ag–Cu–Sn alloys with different composition. The data were evaluated by means of an extended Redlich–Kister–Muggianu polynomial fit for substitutional solutions. The minimum and maximum in the quaternary system were also calculated. It was found that the maximum integral enthalpy of mixing (13,310 J/mol at 41 at.% Ag) occurs in the binary Ag–Ni system while the minimum integral enthalpy of mixing (−21,390 J/mol at 61 at.% Ni) occurs in the binary Ni–Sn system. Moreover the experimental data were compared to values calculated by different extrapolation models based on binary data.

The intent of this work is to investigate thermal stability, microstructure, and electrical properties of thin Hf6Ta2O17 high-k gate dielectrics. X-ray diffraction and transmission electron microscopy analysis reveal that an as-deposited Hf6Ta2O17 film is amorphous with a ∼1-nm interfacial layer. After a 1000 °C anneal, the film is a mixture of orthorhombic-Hf6Ta2O17 and monoclinic HfO2 with a thicker interfacial layer. Uniform Hf and Ta Auger depth profiles are observed for as deposited and annealed films. Secondary ion mass spectrometry (SIMS) analysis shows Hf and Ta profiles are unchanged following the 1000 °C anneal, indicating good thermal stability. There is, however, a clear indication of Si up-diffusion into Hf6Ta2O17, particularly after annealing at 1000 °C. No Hf or Ta is found in the Si substrate. Well-behaved capacitance-voltage curves and low leakage current characteristics were obtained for Mo/ Hf6Ta2O17 capacitors for as-deposited and 1000 °C annealed films. A flatband voltage (Vfb) shift towards negative voltage is observed for the annealed film when compared to the as-deposited film, indicating the presence of more positive charge, or less negative charge. Furthermore, capacitance-voltage stress measurements were performed to study charge trapping behaviors. A smaller Vfb shift is observed for as deposited (<10 mV) versus the 1000 °C annealed (30-40 mV) Hf6Ta2O17, indicating more charge trapping after the high temperature anneal.

The electromigration-induced failure in flip-chip eutectic SnPb solder joints with a 10-μm-thick Cu under-bump metallization (UBM) was studied without the effect of current crowding in the solder region. The current crowding occurred inside the UBM instead of in the solder joint at the current density of 3.0 × 104 A/cm2 because of the spreading of current in the very thick Cu UBM. In these joints, the failure occurred through a two-stage consumption of the thick Cu UBM in the joint where electrons flowed from the chip to the substrate. In the first stage, the Cu UBM dissolved layer by layer rather uniformly across the entire Cu UBM–solder interface. In the second stage, after half of the Cu UBM was dissolved, an asymmetrical dissolution of Cu UBM took place at the corner where electrons entered from the Al interconnect to the Cu UBM. Experimental observation of dissolution steps of the 10-μm-thick Cu UBM is presented. The transition from the first stage to the second stage has been found to depend on the location of current crowding in the flip-chip joints as the UBM thickness changes during the electromigration test. The current distribution in the flip-chip solder joints as a function of UBM thickness was simulated by three-dimensional finite element analysis. The dissolution rate of Cu UBM in the second stage was faster than that in the first stage. The mechanism of electromigration-induced failure in the flip-chip solder joints with a 10-μm-thick Cu UBM is discussed.