Nanocrystalline (NC) Cu samples were synthesized by means of surface mechanical attrition treatment, from which a layer of NC structure was formed on a coarse-grained Cu plate. Low-amplitude oscillating wear/fretting behaviors of the NC Cu samples were investigated under oil lubrication in comparison with those of as-annealed coarse-grained Cu samples. It was found the NC Cu possesses a markedly enhanced wear resistance and a higher friction coefficient relative to the coarse-grained Cu. A continuous metal transfer layer is formed on the mating ball after fretting against the NC Cu, while no material transfer occurs for the as-annealed Cu. The effects of experimental parameters and the hardness of Cu samples on the formation of a transfer layer have been systematically investigated. The transfer layer is evidenced to play an important role in the enhanced wear resistance of the NC Cu, but it has a trivial effect on its high friction coefficient.

Refractory materials such as carbon possess properties that make joining them difficult. In this work, bonding of a carbon–carbon composite is achieved by employing self-sustained, oxygen-free, high-temperature combustion reactions. The effects of several parameters, such as the composition of the reaction media, and the values of the applied current and pressure, on the mechanical strength of the joint were investigated. It was found that the C–C composite possesses a high activity with the reactive media layer, the level of electrical current used to initiate the reaction and the applied pressure do not need to be excessive to obtain a strong joint. Some aspects of the joining mechanism are discussed in detail.

The effect of rapid microwave heating has so far been evaluated mainly by comparing the state of materials before and after microwave exposure. Yet, further progress critically depends on the ability to follow the evolution of materials during ultrafast heating in real time. We describe the first in situ time-resolved monitoring of solid-state phase transitions during microwave heating of metallic powders using wide-angle synchrotron radiation diffraction. Single-phase Al–Cu–Fe quasicrystal powders were obtained by microwave heating of nanocrystalline alloy precursors at 650 °C in <20 s.

Chemical solution deposition has been used to fabricate continuous ultrathin lead lanthanum zirconate titanate (PLZT) films as thin as 20 nm. Further, multilayer capacitor structures with as many as 10 dielectric layers have been fabricated from these ultrathin PLZT films by alternating spin-coated dielectric layers with sputtered platinum electrodes. Integrating a photolithographically defined wet etch step to the fabrication process enabled the production of functional multilayer stacks with capacitance values exceeding 600 nF. Such ultrathin multilayer capacitors offer tremendous advantages for further miniaturization of integrated passive components.

The elastic deformation contribution can significantly affect the measurement of the strain-rate sensitivity (SRS) of the plastic flow stress by indentation methods. In this paper, the effect of such elastic contribution is critically analyzed using an extension of a previous treatment developed by the authors for the elastic effects on the indentation of strain-hardening materials [J. Alkorta et al., J. Mater. Res.20, 432 (2005)]. The analytical model is calibrated and validated through finite element calculations. The results show that when the elastic contribution to the total deformation is not negligible then the measured SRS is significantly lower than the real one. A satisfactory correction factor for the apparent SRS exponent is proposed based on parameters directly accessible to instrumented indentation test results.

Fe–Ni alloy cluster-assembled films were obtained by a plasma–gas-condensation-type cluster-deposition method. We studied the magnetic and electrical properties of these assemblies prepared on an electrically grounded substrate [bias voltage (Va) = 0 kV] and on a negatively biased substrate (Va = −20 kV). The packing density and saturation magnetization per volume, Ms, are much larger for the assemblies prepared at Va = −20 kV than those prepared at Va = 0 kV, while the magnetic coercivity, Hc, and electrical resistivity, ρ, are much lower for the assemblies prepared at Va = −20 kV than those prepared at Va = 0 kV. For Ni-rich Fe–Ni alloy cluster-assembled films obtained at Va = −20 kV, the Hc values can become smaller than 160 A/m (the precision limit of our superconducting quantum interference device magnetometer) by adjusting the initial cluster size. The magnetic and electrical properties of Fe–Ni cluster-assembled films are much improved in comparison with those of pure Fe cluster-assembled films.

A new type of Ti–Si–C–N coatings deposited on high-speed steel substrate by means of pulsed direct current (dc) plasma-enhanced chemical vapor deposition was investigated. The as-deposited coatings were characterized systematically by using energy-dispersive x-ray spectroscopy, x-ray diffraction (XRD), transmission electron microscopy (TEM), and microhardness with particular attention paid to the microstructure of the coatings. It has been shown that C content has a profound effect on the microstructure and hardness of coatings. TEM and XRD analyses revealed that these coatings consist of the dominate Ti(C, N) with a silicide (TiSi2, Si3N4, or SiC, depending on the C content in the coatings). The crystallite sizes are in the range of 8–35 nm, which decrease with increasing C content. The Ti–Si–C–N coatings with high C content (25.2–38.6 at.%) possess superhardness (41–48 GPa). This can be attributed to the grain refinement/grain boundary hardening and dispersion hardening of the hard, nanosized crystalline Si3N4 or SiC formed in the deposition.

Accurate determination of the “zero point,” the first contact between an indenter tip and sample surface, has to date remained elusive. In this article, we outline a relatively simple, objective procedure by which an effective zero point can be determined accurately and reproducibly using a nanoindenter equipped with a continuous stiffness measurement option and a spherical tip. The method relies on applying a data shift, which ensures that curves of stiffness versus contact radius are linear and go through the origin. The method was applied to fused silica, sapphire single crystals, and polycrystalline iron with various indenter sizes to a zero-point resolution of ≈2 nm. Errors of even a few nanometers can drastically alter plots and calculations that use the data, including curves of stress versus strain.

Magnesium hafnium tungstate [MgHf(WO4)3] was synthesized by high-energy ball milling followed by calcination. The material was characterized by variable- temperature neutron and x-ray diffraction. It crystallized in space group P21/a below 400 K and transformed to an orthorhombic structure at higher temperatures. The orthorhombic polymorph adopted space group Pnma, instead of the Pnca structure commonly observed for other A2(MO4)3 materials (A = trivalent metal, M = Mo, W). In contrast, the monoclinic polymorphs appeared to be isostructural. Negative thermal expansion was observed in the orthorhombic phase with αa = −5.2 × 10−6 K−1, αb = 4.4 × 10−6 K−1, αc = −2.9 × 10−6 K−1, αV = −3.7 × 10−6 K−1, and αl = −1.2 × 10−6 K−1. The monoclinic to orthorhombic phase transition was accompanied by a smooth change in unit-cell volume, indicative of a second-order phase transition.

Residual stress profiles were introduced in sodium aluminosilicate glass disks using an ion-exchange process. They were fractured in two loading conditions: indentation and biaxial flexure. The fractal dimension of the macroscopic crack branching pattern called the crack branching coefficient (CBC), as well as the number of fragments (NOF) were used to quantify the crack patterns. The fracture surfaces were analyzed to determine the stresses responsible for the crack branching patterns. The total strain energy in the body was calculated. The CBC was a good measure of the NOF. They are directly related to the tensile strain energy due to the residual stress profile for fractures due to indentation loading. However, in general for materials with residual stresses, CBC (or NOF) is not related to the strength or the stress at fracture, or even to the total stored tensile strain energy. Instead, the CBC appears to be related, in a complex manner, to the distribution of stresses in the body. Therefore, in general, the characterization of the CBC of fractured materials cannot be used to ascertain the prior stress distribution.

The effects of the Zr/Ti ratio on the electrical properties of lead zirconate titanate (PZT) thick films prepared by the aerosol deposition (AD) process were investigated to optimize the electrical properties of the thick film. The Zr/Ti ratio was varied among 45/55, 52/48, and 60/40, and the post-annealing temperature was varied from 500 to 900 °C. Microscopic examination of the as-deposited films revealed crack-free and dense microstructures with a thickness of 10 μm. The annealed films showed markedly improved electrical properties in comparison with the as-deposited films with increasing post-annealing temperature. With increasing Zr/Ti ratio, the remnant polarization and coercive field decreased. The dielectric constant and piezoelectric coefficient, d33, were highest for the PZT 52/48 film. This film annealed at 900 °C exhibited the best overall combination of electrical properties, with a dielectric constant, remnant polarization, and piezoelectric coefficient of 1320, 31.1 μC/cm2, and 150 pC/N, respectively.

To impart machinability to hard and brittle AlN ceramics without losing their high thermal conductivity, a homogeneous dispersion of fine BN particles in an AlN matrix was investigated. A homogeneous dispersion of BN particles was obtained by pressureless sintering of turbostatic BN-coated AlN nanocomposite powder (AlN–BN nanocomposite powder), which was prepared by reducing and heating AlN particles containing a mixture of boric acid, urea, and carbon. Though AlN is slightly oxidized by boric acid during the reduction, the addition of carbon reduced the oxygen content of the AlN–BN composite powder by carbothermal reduction of the oxidized AlN particles. As a result, the thermal conductivity of the sintered material increased with decreasing oxygen content of the nanocomposite powder. AlN–BN nanocomposites containing more than 20 vol% BN showed high strength, machinability, and relatively high thermal conductivity in comparison with the conventional microcomposites.

Indentations were performed on silicon using a Berkovich indenter at loads up to 12 mN, at temperatures from 20 to 135 °C. Transmission electron microscopy revealed crystalline silicon phases in the residual indentation imprint at and above 35 °C. Also, the first reconfirmation of the occurrence of Si-VIII during unloading was observed at temperatures of 100 and 125 °C. Interestingly, at 125 °C a cavity was also observed, and an unidentifiable phase was observed at 135 °C. The observations show the strong effect of temperature on pressure-induced phase transformation in silicon.

The high local temperature in flip-chip solder joints of microprocessors has raised concerns that the solder, a low melting temperature alloy, might locally liquefy and consequently cause failure of the microprocessors. This article reports a highly interesting electromigration behavior when the solder is in the molten state. A 6.3 × 103 A/cm2 electron current was applied to molten Sn3.5Ag solder at 255 °C through two Cu electrodes. The high current density caused rapid dissolution of the Cu cathode. The dissolved Cu atoms were driven by electrons to the anode side and precipitated out as a thick, and sometimes continuous, layer of Cu6Sn5. The applied current caused the dissolution rate of the Cu cathode to increase by one order of magnitude. A major difference between the electromigration in the solid and molten state was identified to be the presence of different countering fluxes in response to electromigration. For electromigration in the molten state, the back-stress flux, which was operative for electromigration in the solid state, was missing, and instead a countering flux due to the chemical potential gradient was present. An equation for the chemical potential gradient, dμ/dx, required to balance the electromigration flux was derived to be dμ/dx = N°z*eρJ, where N° is Avogadro’s number, z* is the effective charge of Cu, e is the charge of an electron, ρ is the resistivity of the solder, and J is the electron current density.

Cu–Zn is an important binary alloy system. In the interested temperature range from 300 to 1500 K, there are eight phases, liquid, Cu, β, β′, γ, δ, ϵ, and Zn phases. The thermodynamic descriptions of the Cu–Zn system are reassessed using the CALPHAD method. A new description of liquid phase and simplified description of body-centered cubic (bcc) phase are proposed. Good agreement has been found among the calculated thermodynamic properties, phase diagram, and the experimental information.

The electromigration behavior of the Cu/Au/SnAgCu/Cu combination was investigated under 103 A/cm2 of current stressing at ambient temperature. The Au layer, when it acts as a cathode, was consumed continuously, and no significant compound was found at the interface. Meanwhile, Cu6Sn5 was formed at the anodic Cu layer, and the thickness of the compound increased with increasing time. The Au atoms were found to be trapped in Cu6Sn5 within the solder matrix. The AuSn4 compound precipitated while attaching to Cu6Sn5 at the Cu6Sn5/solder interface. The thermomigration effect was found to be insignificant in this work as no obvious reaction occurred at the cathode/anode sides or in the solder matrix without current stressing.

Nanostructured tungsten trioxide films were fabricated with the technique of glancing angle deposition (GLAD) in a thermal evaporation chamber with a base pressure of 1.3 × 10−4 Pa. Films were deposited at vapor incidence angles of 0°, 20°, 40°, and 50° with film thickness varying between 160 and 200 nm, as determined by spectroscopic ellipsometry. After deposition, samples were heated for 1 h in air at 400 °C and were subsequently intercalated with small amounts (5 to 15 nm) of lithium by dry lithiation, a technique developed in our laboratory. Compared with our previous work on as-deposited nanostructured films, these samples showed significantly enhanced coloration in the infrared region. It was found that the films exhibited an absorption- based coloration in the lower wavelengths as well as an increased reflection in the infrared region. Morphological investigation by atomic force microscopy (AFM) showed grain agglomeration and increased surface roughness upon heating. Our studies further indicate that grain agglomeration significantly contributes to the superior coloration properties of the films.

Near-infrared (NIR)-absorbing nanoparticles synthesized by the reduction of tetrachloroauric acid (HAuCl4) using sodium sulfide (Na2S) exhibited absorption bands at ∼530 nm and at the NIR region of 650−1100 nm. A detailed study on the structure and microstructure of as-synthesized nanoparticles was reported previously. The as-synthesized nanoparticles were found to consist of amorphous AuxS (x = ∼2), mostly well mixed within crystalline Au. In this work, the optical properties were tailored by varying the precursor molar ratios of HAuCl4 and Na2S. In addition, a detailed study of composition and particle-size effects on the optical properties was discussed. The change of polarizability by the introduction of S in the form of AuxS (x = ∼2) had a significant effect on NIR absorption. Also, it was found in this work that exposure of these particles to NIR irradiation using a Nd:YAG laser resulted in loss of the NIR absorption band. Thermal effects generated during NIR irradiation had led to microstructural changes that modified the optical properties of particles.