We report on the growth of Mg-rich cubic (Mg,Zn)O nanowires using a catalysis-driven molecular-beam-epitaxy method. Nanowires were grown on both Si and Al2O3 substrates coated with a nominally 2-nm-thick layer of Ag. The (Mg,Zn)O nanowires were grown with a Zn and Mg cation flux, with an O2/O3 mixture serving as the oxidizing species. The growth temperature was 400 °C. Under these conditions, nanowires were observed to grow on the Ag sites. The nanowire diameter was on the order of 90 nm. (Mg,Zn)O nanowires as long as 2 μm were realized. High-resolution transmission electron microscope imagery shows the nanowires had single-phase cubic rock salt structure (Mg,Zn)O with a growth direction along the [100]. The presence and compositional distribution of Mg and Zn in the single nanowire were confirmed using a compositional line-scan, profiled across the nanowire, by energy dispersive spectrometry with scanning transmission electron microscopy.

Two-dimensional layered ceramics, highly anisotropic materials in terms of structure and properties, were used to produce polymer-covered metal nanorods and metal microcrystals. The procedure took advantage of the intrinsic planar, layered ordering of the metal cations suitable to be reduced and could be further used to engineer one-dimensional metal alloy nanostructures by appropriate doping of the initial layered ceramic lattice with suitable cationic species. The procedure involved the formation in an intermediate step of a polymer-intercalated ceramic nanocomposite, highly porous to the diffusion of the polymerizable reducing agent, pyrrole. Two structurally similar layered bismuthates, Bi2Sr2CaCu2O8+δ and Bi6Sr2CaO12 and a partially Rh-substituted ceramic, Bi4Rh2Sr2CaO12 were used as the precursor layered ceramics and the reducible metal cations were Cu2+, Bi3+, and Rh3+, respectively. The formation of the polymer-covered metal nanorods and metal microcrystals took place at relatively high temperatures of reaction (325 °C) and long reaction times (10–12 days).

We report the use of low-energy nitrogen ion beams to form ultra-thin (<2 nm) layers of AlNx to act as tunnel barriers in Nb/Al–AlNx/Nb Josephson junctions. We fabricated reproducible, high-quality devices with independent control of the ion energy and dose, enabling exploration of a wide parameter space. Critical current density Jc ranged from 550 to 9400 A/cm2 with subgap-to-normal resistance ratios from 50 to 12.6. The spatial variation of ion-current density was roughly correlated with Jc over a large-area on a Si substrate. The junctions were stable on annealing up to temperatures of at least 200 °C. This technique could be applied to form other metal nitrides at room temperature for device applications where a high degree of control is desired.

Highly pure Co nanocrystalline powders were prepared by high-energy ball milling under the condition that all operations on the powders were performed in the glovebox filled with highly purified argon gas. A series of annealing experiments at different temperatures were carried out to investigate grain growth in the milled powders. The as-milled and annealed microstructures were observed and analyzed with transmission electron microscopy (TEM), high-resolution TEM, high-resolution scanning electron microscopy, and x-ray diffraction methods. Characteristics of the incontinuous grain growth in the milled nanocrystalline powders were found. It is considered by the authors that the sharp increase in nanograin size in certain intermediate-temperature region is a result of accelerated grain growth promoted by the stored energy as a supplied driving force, and through a particular dominant mechanism of nanograin rotations in contrast to grain boundary migration in polycrystalline materials.

Instrumented indentation is often used in the study of small-scale mechanical behavior of “soft” matters that exhibit viscoelastic behavior. A number of techniques have recently been proposed to obtain the viscoelastic properties from indentation load–displacement curves. In this study, we examine the relationships between initial unloading slope, contact depth, and the instantaneous elastic modulus for instrumented indentation in linear viscoelastic solids using either conical or spherical indenters. In particular, we study the effects of “hold-at-the-peak-load” and “hold-at-the-maximum-displacement” on initial unloading slopes and contact depths. We then discuss the applicability of the Oliver–Pharr method (Refs. 29, 30) for determining contact depth that was originally proposed for indentation in elastic and elastic-plastic solids and recently modified by Ngan et al. (Refs. 20–23) for viscoelastic solids. The results of this study should help facilitate the analysis of instrumented indentation measurements in linear viscoelastic solids.

Using depth-sensing indentation with sub-nanometer displacement resolution, the plastic deformation of a range of materials, including a metallic glass, amorphous selenium, Ni3Al, pure Nb, Al, Cu, and Zn metals, and an Al-Mg alloy, has been investigated at room temperature. In amorphous selenium, even the sub-nanometer displacement resolution of the nanoindentation technique cannot reveal any strain burst during deformation at room temperature. In all other metals studied, what may appear to be smooth load-displacement curves at macroscopic scale during indentation deformation in fact turn out to consist of a continuous series of random bursts of the nanometer scale. The occurrence probability of the bursts is found to decrease at increasing burst size. In all of the crystalline metals and alloys studied, the size distribution of the strain bursts seems to follow an exponential law with a characteristic length scale. The absence of the self-organized critical behavior is likely a result of the small size of the strained volume in the nanoindentation situation, which gives rise to a constraint of a characteristic strain. In the metallic glass sample, due to the limited range of the burst sizes encountered, whether the deformation bursts follow an exponential or a power-law behavior corresponding to self-organized criticality is inconclusive. From a theoretical viewpoint based on the Shannon entropy, the exponential distribution is the most likely distribution at a given mean burst size, and this is thought to be the reason for its occurrence in different materials.

Agglomerates of aligned crystals of CaxCo2O4 with a layer of CoO2 were grown using a chloride flux technique, and their thermoelectric properties in air were determined. The agglomerates take the form of a very thin flakelike cluster of crystals with a typical size of almost 3 × 2 × 0.07 mm. The values of thermoelectric power along the ab-plane are larger than 200 μV K−1 at temperatures above 873 K and reach almost 300 μV K−1 at 973 K. The temperature dependence of the electrical resistivity along the ab-plane shows bends around 450 and 825 K, and the ln ρab−T−1 curve followed an Arrhenius-type behavior below 450 K. Temperature dependence of thermal conductivity indicated that stacking faults along the c axis induce phonon scattering like that in a misfit-layered structure. The effect of the CoO2 layer on thermoelectric performance is discussed in comparison with related compounds.

Sn–3.5Ag solder bumps were formed on electroless Ni/immersion Au (Ni/Au) and organic solderability preservative (OSP) surface-finished bond pads, respectively. The shear strength of the solder bumps was measured as a function of reflow steps. Fracture surfaces and interfacial microstructures were investigated by scanning electron microscope. The shear strength of Ni/Au samples increased up to the seventh reflow step and subsequently decreased after the tenth reflow step. Spalling of Ni3Sn4 intermetallic compounds (IMCs) and the P-rich Ni layer strengthened and weakened the bond, respectively. For OSP samples, although Cu6Sn5 IMCs grew as the reflow step was repeated, no remarkable change in shear strength was observed. Interfacial fractures of OSP samples occurred at the interface between Cu6Sn5 IMC and Cu3Sn IMC. Fracture surfaces of OSP samples showed concave pits that consisted of a Cu3Sn bottom and an Sn wall. The pits were formed by separation of Cu6Sn5 IMC from Cu3Sn IMC and the molten Sn channel between the Cu6Sn5 IMC grains.

Cobalt nanoparticles were synthesized on silica thin films by heat treating Co/silica films spun on thermally oxidized Si substrates. The as-deposited films were calcined in vacuum (∼0.03 Torr) for 2 h at 500 °C, followed by reduction in hydrogen at 650 °C for up to 15 h. The reduction process is characterized as one of time-dependent evolution of nanoparticles in both physical appearance and phase nature, eventually leading to the formation of well-dispersed Co nanoparticles, as ascertained by x-ray photoelectron spectroscopy and scanning electron microscopy. Slow conversion of Co ions into metallic Co observed in this study is ascribed to the absence of a Co3O4 phase that forms predominantly during calcination in air. Atomic force microscopy revealed a marked increase in the surface roughness of the film due to the development of nanoparticles. A distinct duplex-layer structure was observed in the reduced film, which consisted of the upper layer laden with nanoparticles and the lower layer essentially particle-free. The growth of the upper layer appears to be controlled by the upward diffusion of Co2+ in the film during the reduction process.

Among many Sn-based intermetallics, Cu6Sn5 (η and η′) is ubiquitous in modern solder interconnects. Using the published structural models of η and η′ and also related structures, the total energies and equilibrium cohesive properties are calculated from first-principles employing electronic density-functional theory, ultrasoft pseudopotentials, and both the local density approximation (LDA) and the generalized gradient approximation (GGA) for the exchange-correlation energy. The accuracy of our calculations is assessed through comparisons between theoretical results and experimental measurements for lattice parameters, elastic properties, and formation and transformation energies. The ambient-temperature experimental lattice constants of η and η′ are found to lie between the LDA and GGA level calculated zero-temperature lattice constants. The Wyckoff positions in the structural models of η and η′ agree very well with the ab initio results. The calculated formation energy of η′ lies between −3.2 and −4.0 kJ/mol, which is more positive by about 3 to 4 kJ/mol compared to reported experimental data obtained by solution calorimetry. Our systematic differential scanning calorimetry (DSC) experiments show that the η′ → η transformation enthalpy is 438 ± 18 J/mol, which is about 66% higher than the literature value. In view of our DSC results on heating and cooling, the nature of η′ → η and η → η′ is discussed. Our experimental bulk modulus of η and η′, and the heat of η′ → η transformation agree very well with the ab initio total energy calculations at the GGA level. Based on these results, we conclude that other isotropic elastic moduli (Young’s modulus, shear, and Poissons ratio) of η and η′ phases measured by pulse-echo technique are representative of their actual properties. The scatter in experimental elastic constants in the literature may be attributed to various factors, such as the measurement technique (pulse-echo versus nanoindentation), type of specimen (bulk, Cu6Sn5-layer in diffusion couple, thin-film), and anisotropy effects (particularly in Cu6Sn5-layer in diffusion couples).

The interfacial reactions between solders and under bump metallization (UBM) have been of great interest recently in flip chip technology. Intermetallic compounds (IMCs), i.e., (Cu,Ni)6Sn5 and (Ni,Cu)3Sn4, usually formed between solders and UBM. To fully understand the interfacial reactions and phase transformation phenomenon, a suitable phase diagram concerning solders, IMCs, and UBM materials is required. In particular, a Sn-rich phase region in the Sn–Cu–Ni ternary diagram is very critical in determining the concentration tendency of x and y values in (Ni1−x,Cux)3Sn4 and (Cu1−y,Niy)6Sn5 compounds. In this study, ternary Sn–Cu–Ni alloys were prepared and annealed at 240 °C. Three equilibrium phases, Sn, Ni3Sn4, and Cu6Sn5, were identified by x-ray diffraction analysis and also showed in backscattered electron imaging. Using electron probe microanalysis quantitative analysis, three acme compositions of the ternary region in the Sn–Cu–Ni isotherm near the Sn-rich corner were determined as 98.5 at.% Sn, (Ni0.80, Cu0.20)3Sn4 and (Cu0.59,Ni0.41)6Sn5. In addition, the solubility of Cu and Ni in (Ni,Cu)3Sn4 and (Cu,Ni)6Sn5 compounds was evaluated. Finally, the isothermal section of the ternary Sn–Cu–Ni system at 240 °C was proposed on the basis of experimental results in this study.

Ultra-thin ZrO2 and HfO2 dielectric films grown by atomic layer deposition (ALD) are quite promising materials for gate dielectric applications in future transistors, and they exhibit significantly different as-grown microstructures: polycrystalline and amorphous phases, respectively. However, under the identical deposition conditions, both metal oxides show surprisingly similar capacitance–voltage (C–V) characteristics as a function of film thickness, implying that the identities and densities of fixed charge and bulk trapping charge are similar. Factors other than the film microstructure, such as concentration of impurities incorporated during the film deposition, are believed predominantly to control important C–V characteristics. Only the dielectric constant appears to depend significantly on the identity of the dielectric material. It is found that the dielectric constant of ALD-HfO2 (∼20) is significantly lower than that of ZrO2 (∼30) due to the differences in microstructure and also atomic density of the film. In terms of the leakage current characteristics, the effective potential barrier heights between Pt and these two dielectric films are identical (∼2.3 eV) within the experimental uncertainty. Implications for the electrode/dielectric interface electronic structure are discussed.

Wavelength dependence was observed in the ultraviolet (UV) irradiation-assisted crystallization of alkoxy-derived ZrO2 thin films. The surface grains of thin films deposited on Si(100) substrates became enlarged by UV irradiation using an ultrahigh-pressure mercury lamp. The crystallinity of thin films deposited on Si(100) substrates was improved by UV irradiation using a low-pressure mercury lamp. The reaction using the ultrahigh-pressure mercury lamp depended on the substrate type.

Thin films of SiO2–TiO2 composite oxides with various SiO2:TiO2 compositions were prepared by the sol-gel method, using tetraethylorthosilicate (TEOS) and titanium tetraisopropoxide (TTIP) as precursors. The composition, crystal structure, and chemical bonding configuration of the as-deposited and annealed SiO2–TiO2 thin films were analyzed using Rutherford backscattering spectrometry (RBS), glancing incident angle x-ray diffraction (GIAXRD) and Fourier transform infrared spectroscopy (FTIR), respectively. Optical properties of the films were characterized by spectroscopic ellipsometry and ultraviolet-visible spectrophotometry. The Si/Ti ratios in the SiO2–TiO2 films agree with the TEOS/TTIP molar ratio in the sol-gel precursor. When the TEOS/(TEOS + TTIP) ratio is greater than 40%, the SiO2–TiO2 thin films remain amorphous (without formation of TiO2 crystalline phase) after annealing at temperatures as high as 700 °C. FTIR spectra indicate that the quantity of Si–O–Ti bonding can be maximized when the TEOS:TTIP in the precursor is 80%:20%. The refractive index of the SiO2–TiO2 films increases approximately linearly to the mixing ratio of TTIP/(TEOS + TTIP). However, SiO2-rich films possess higher ultraviolet-visible transmittance than the TiO2-rich films. The modification of microstructure and chemical bonding configuration in the SiO2–TiO2 films by the composition and its influence on the optical properties are discussed.

The indentation size effect of pure iron samples with various pre-plastic tensile strains has been experimentally investigated and analyzed. With the increase in the strain, the indentation size effect of iron samples becomes weak, accompanied by the multiplication of the statistically stored dislocations. All of the hardness (H) versus indentation depth (h) curves fit the strain-gradient plasticity model for indentation of Nix and Gao well. Two fitting parameters, the hardness in the limit of infinite depth (H0) and the characteristic length (h*), were obtained for each curve. The hardness (H0) of iron samples can also be estimated as the microhardness (H) at a very large depth, h ≅ 10h*. Both the fitted H0 and the measured H0′ increase linearly with the tensile yield stress σy of iron samples, indicating a dependence of H0 on the statistically stored dislocation density through σy. Furthermore, 1/√h* shows a linear increase with the tensile yield stress σy, which also agrees qualitatively with the general prediction of the Nix and Gao theory. Therefore, our experiments and analysis demonstrate that the strain-gradient plasticity model for indentation of Nix and Gao can interpret the indentation size effect with satisfied precision.

“Nanoscale Morphology and Indentation of Individual Nacre Tablets from the Gastropod Mollusc Trochus Niloticus” [J. Mater. Res. 20, 2400 (2005)]