Bulk metallic glass (BMG) formations in Co- and Fe-based alloy systems are investigated by using our cluster line approach in combination with minor alloying principle. Basic ternary alloy compositions in Co–B–Si, Fe–B–Y, and Fe–B–Si systems are first determined by cluster lines defined by linking special binary clusters to third elements. Then the basic ternary alloys are further minor alloyed with 3 to 5 at.% Nb to improve glass-forming abilities (GFAs) and ϕ3 mm BMGs are formed in (Co8B3–Si)–Nb and (Fe8B3–Y)–Nb but not in (Fe8B3–Si)–Nb, TM8B3 (TM = Fe, Co) being the most compact binary cluster. The BMGs are expressed approximately with a unified simple composition formula: (TM8B3)1M1, M = (Si, Nb) or (Y, Nb). Finally, mutual Fe and Co substitutions further improve the GFAs as well as the soft magnetic properties, e.g., Is reaching 0.98 T and Hc < 6 A/m for the Co–Fe–B–Si–Nb BMGs. Using the (cluster)1(glue atom)1 model, a new ternary BMG Fe8B3Nb1 is obtained.

Surface modification of the elastomer polydimethylsiloxane (PDMS) by exposure to oxygen plasma for four minutes creates a thin, stiff film. In this study, the thickness and mechanical properties of this surface-modified layer were determined. Using the phase image capabilities of a tapping-mode atomic force microscope (AFM), the surface-modified region was distinguished from the bulk PDMS; specifically, it suggested a graded surface layer to a depth of about 200 nm. Load-displacement data for elastic indentation using a compliant AFM cantilever was analyzed as a plate bending on an elastic foundation to determine the elastic modulus of the surface (37 MPa). An applied uniaxial strain generated a series of parallel nanocracks with spacing on the order of a few microns. Numerical analyses of this cracking phenomenon showed that the depth of these cracks was in the range of 300–600 nm and that the surface layer was extremely brittle, with toughness in the range of 0.1– 0.3 J/m2.

An atomic force microscope (AFM) was used to characterize the deformation behavior of amorphous Si (a-Si) nanostructures subjected to monotonic and cyclic loading. The sample geometry was specially designed (in the form of elbow) using finite element modeling for the purpose of these tests, and the samples were grown by glancing angle deposition. When deformed monotonically at room temperature, the a-Si specimens exhibited a nonlinear force–displacement response at forces larger than a critical force, a phenomenon not observed in bulk silicon. A fatigue testing methodology based on the use of the AFM was established. The fatigue life of the a-Si specimens was observed to increase by five orders of magnitude with a 50% reduction in the applied force amplitude. It was verified that this delayed failure is caused by progressive damage accumulation during cyclic loading. These results are compared with literature data obtained from micron-size specimens.

The microstructures and mechanical properties of Mg–6Zn–5Al–4Gd–1RE (RE = Ce or Y) alloys were investigated. The addition of Ce or Y obviously refines the grain size for the Mg–6Zn–5Al–4Gd-based alloy, while the Y element has a better refining effect. The Ce and Y show different grain-refining mechanisms: Ce addition mostly promotes the growth of secondary dendrite, while Y addition mainly increases the heterogeneous nucleation sites. The hardness-versus-aging time curves indicate that all the alloys have excellent aging-hardening behavior, but the response to maximum hardness was delayed by the Ce or Y addition. The microstructure observation of the peak-aged alloys indicated a large number of nanocrystalline τ-Mg32(Al, Zn)49 precipitates in the matrix. The Y addition is beneficial to improve the mechanical properties, and the alloy has optimal values. However, the Ce addition decreases the ultimate tensile strength and elongation of the alloy due to formation of a lot of shrinkage porosities.

Upconversion luminescence (UPL) characteristics and effects of Li+ ion on the UPL of ZnWO4:Yb,Er polycrystalline phosphors were investigated. It was shown that introduction of Li+ ions could reduce the calcination temperature by about 200 °C and increase the crystallinity of ZnWO4:Yb,Er by a liquid-phase sintering process via formation of Li2WO4 and other intermediates. UPL efficiency is remarkably promoted by Li+ ions. Moreover, the UPL spectrum of Li+-doped ZnWO4:Yb,Er presents a red shift, and the strongest peak position shifts from 553 to 559 nm. These can be attributed to a shift in the 4f level barycenter to lower energy, which results from lowering of the symmetry of the crystal field around Er3+.

The electromigration and thermomigration behavior of eutectic tin-lead flip chip solder joints, subjected to currents ranging from 1.6 to 2.0 A, at ambient temperatures above 100 °C, was experimentally and numerically studied. The temperature at the chip side was monitored using both a temperature coefficient of resistance method and a thermal infrared technique. The electron wind force and thermal gradient played the dominant role in accelerated atomic migration. The atomic flux of lead due to electromigration and thermomigration was estimated for comparison. At the current crowding region, electromigration induced a more serious void accumulation as compared with thermomigration. Also, because of different thermal dissipations, a morphological variation was detected at different cross-sectional planes of the solder joint during thermomigration.

Extensive experimental research work has been carried out to investigate precipitation peculiarities in Mg–Zn–Sn-based alloys during aging at different temperatures. This in-depth research was conducted on Mg–4.4wt%Zn–4.0wt%Sn–0.6wt%Y and Mg–4.4wt%Zn–4.4wt%Sn–1.1wt%Sb using x-ray diffraction (XRD), transmission electron microscopy (TEM) including high-resolution TEM, and scanning electron microscopy (SEM) equipped with an energy-dispersive x-ray spectrometer (EDS). It was found that, first, a hexagonal close-packed (hcp)-MgZn2 phase nucleates and grows in the form of needles having coherent interphase boundaries with α-Mg matrix. Then the face-centered cubic (fcc)-Mg2Sn-phase nucleates heterogeneously, mainly at the tips of MgZn2 needles. A very certain mutual orientation of crystal lattices of MgZn2, Mg2Sn, and α-Mg matrix was revealed. The orientation of Mg2Sn precipitates is perpendicular to that of MgZn2 needles. They grow in the form of plates parallel to the basal planes of α-Mg matrix. Two-phase T-like particles are very typical of alloys aged for 1 to 16 days at 175 to 225 °C. The width/length ratio of MgZn2 needles inside T-like particles differs substantially from that found in single needles. The elastic/surface energy balance of needles and its influence on the morphology and coarsening behavior has been analyzed.

Microstructure and hardness evolution of arc-evaporated single-phase cubic Al0.56Cr0.44N and Al0.68Cr0.32N coatings have been investigated after thermal treatment in Ar atmosphere. Based on a combination of differential scanning calorimetry and x-ray diffraction studies, we can conclude that Al0.56Cr0.44N undergoes only small structural changes without any decomposition for annealing temperatures Ta ⩽ 900 °C. Consequently, the hardness decreases only marginally from the as-deposited value of 30.0 ± 1.1 GPa to 29.4 ± 0.9 GPa with Ta increasing to 900 °C, respectively. The film with higher Al content (Al0.68Cr0.32N) exhibits formation of hexagonal (h) AlN at Ta ⩾ 700 °C, which occurs preferably at grain boundaries as identified by analytical transmission electron microscopy. Hence, the hardness increases from the as-deposited value of 30.1 ± 1.3 GPa to 31.6 ± 1.4 GPa with Ta = 725 °C. At higher temperatures, where the size and volume fraction of the h-AlN phase increases, the hardness decreases to 27.5 ± 1.0 GPa with Ta = 900 °C.

The deformation behavior of diamondlike carbon (DLC) coatings on silicon substrates induced by Berkovich indentation has been investigated. DLC coatings deposited by a plasma-assisted chemical vapor deposition technique were subjected to nanoindentation with a Berkovich indenter over a range of maximum loads from 100 to 300 mN. Distinct pop-ins were observed for loads greater than 150 mN. However, no pop-out was observed for the loads studied. The top surface of the indents showed annular cracks with associated fragmented material. The cross sections showed up to 20% localized reduction in thickness of the DLC coating beneath the indenter tip. Cracking, {111} slip, stacking faults, and localized phase transformations were observed in the silicon substrate. The discontinuities in the load–displacement curves at low loads are attributed to plastic deformation of the silicon substrate, whereas at higher loads they are attributed to plastic deformation as well as phase transformation.

An amorphous polymer was contacted by a Berkovich indenter using the same loading history but with four different unloading rates following a wide range of load-hold time periods. The strain-rate sensitivity index of the creeping solid was determined at each load-hold period based on two readily determinable parameters, which are the effective contact stiffness and strain rate at the onset of unloading. The measured strain-rate sensitivity index was found to increase with decreasing load-hold period, suggesting that the elastic moduli of the amorphous polymers determined by nanoindentation (together with the true contact area) depends significantly on the selection of the load-hold period. The rheological condition of the creeping solid under constant load changes substantially with time to affect the subsequent unloading recovery process. It is therefore advisable to control not only the unloading strain rate but also the load-hold period when testing time-dependent materials.

Titania coatings with various morphologies were formed on titanium surfaces by hydrothermal treatment using a dilute alkaline solution and evaluated in their hydroxyapatite (HA)-forming abilities in simulated body fluid (1.5SBF) under ultraviolet (UV) irradiation. The HA formation on the titania coating in 1.5SBF was enhanced by UV irradiation. The amount of phosphate groups adsorbed on the titania, after soaking in 1.5SBF for 24 h under UV irradiation, was estimated to be larger than that of calcium ions, whereas that of calcium ions on the titania, after soaking without UV irradiation, was larger than that of phosphate groups. It was suggested that the titania generated much basic Ti–OH groups at its surface by UV irradiation and subsequently adsorbed phosphate groups, such as H2PO4−, resulting in the formation of a new surface rich in the amount of the groups, which eventually enhanced the HA formation in 1.5SBF.

In2−xCoxS3 (x = 0 to 0.1) micropompons (diameters ∼3–4 μm) consisting of ∼10–15-nm-thick randomly self-assembled nanoflakes were synthesized hydrothermally. X-ray study indicated a steady variation of lattice parameter ratio up to 5% Co. Detailed investigations of the Co incorporation in In2S3 were carried out by optical absorbance, room temperature photoluminescence (PL), and electron paramagnetic resonance (EPR) studies. Significant blue shift in the absorbance spectra was noticed due to the crystal-field splitting of Co2+ ions in the host lattice structure. Unlike the visible emission found in undoped In2S3, PL spectra of the Co-doped samples were recognized by a strong ultraviolet emission peak at ∼335 nm, introduced by the t2g level of Co2+ ions, with maximum intensity for 5% Co. Room-temperature and low-temperature EPR spectra revealed octet paramagnetic bands up to 5% Co beyond which a single resonance band appeared.

A new grain-growth mode is observed in thick sputtered copper films. This new grain-growth mode, also referred to in this work as super secondary grain growth (SSGG) leads to highly concentric grain growth with grain diameters of many tens of micrometers, and drives the system toward a {100} texture. The appearance, growth dynamics, final grain size, and self-annealing time of this new grain-growth mode strongly depends on the applied bias voltage during deposition of these sputtered films, the film thickness, the post-deposition annealing temperature, and the properties of the copper diffusion barrier layers used in this work. Moreover, a clear rivalry between this new growth mode and the regularly observed secondary grain-growth mode in sputtered copper films was found. The microstructure and texture evolution in these films is explained in terms of surface/interface energy and strain-energy density minimizing driving forces, where the latter seems to be an important driving force for the observed new growth mode. By combining these sputtered copper films with electrochemically deposited (ECD) copper films of different thickness, the SSGG growth mode could also be introduced in ECD copper, but this led to a reduced final SSGG grain size for thicker ECD films. The knowledge about the thin-film level is used to also implement this new growth mode in small copper features by slightly modifying the standard deposition process. It is shown that the SSGG growth mode can be introduced in narrow structures, but optimizations are still necessary to further increase the mean grain size in features.

Hybrid thick films were deposited on Surlyn, a copolymer of poly(ethylene- co-methacrylic acid) and a common adhesion film for metal surfaces. Hybrid organic–inorganic materials were prepared by a sol-gel process. Methyltriethoxysilane (MTES) with tetraethoxysilane (TEOS), phenyltriethoxysilane (PhTES) with TEOS, and methyltrimethoxysilane (MTMS) with tetramethoxysilane (TMOS) were investigated. The inorganic component was selected to form the network for the film, while the organic component was selected to repel water and fill porosity. The films were deposited on Surlyn and on glass slides. The properties of the films were investigated using attenuated total reflection Fourier transform infrared (FTIR) and Raman spectroscopy. Contact-angle measurements indicated that the contact angle increased from ∼76.5° for Surlyn alone to ∼89.6° for Surlyn coated with MTES.

High-temperature order–disorder transformations in R2T17 and R2T17-M-C intermetallics with R = Pr, Sm, Dy, Tb; T = Co, Fe; and M = Zr, Nb were studied utilizing time-resolved synchrotron x-ray diffraction at the Advanced Photon Source (APS) at the U.S. Department of Energy’s Argonne National Laboratory (Argonne, IL). High-energy synchrotron radiation provides intense, highly penetrating x-rays, which are ideal for in situ studies of phase transformations. Alloying additions are used to stabilize formation of metastable phases; their influence on order recovery was investigated. The experimental setup utilized Debye–Scherrer geometry; specimens were heated at a rate of 10 K/min. Full-profile diffraction patterns collected every 10 s were refined in sequence using the Rietveld method to track changes of lattice parameters and phase assemblages during heating. Sharp changes observed in the evolution of temperature-dependent lattice parameters suggested formation of ordered structure via nucleation and growth. Both 2-17 polymorphs co-existed in light and heavy rare-earth systems at high temperatures. The presence of alloying additions in the solid solution greatly influenced long-range order formation.

Hydrogenation and dehydrogenation of metal hydrides are of great interest because of their potential in on-board applications for hydrogen vehicles. This paper aims to study hydrogen diffusion in metal hydrides, which is generally considered to be a controlling factor of hydrogenation/dehydrogenation. The present work first calculated temperature-dependent hydrogen diffusion coefficients by a theoretical model incorporated with experimental data in a Mg-based system and accordingly the activation energy. The grain size effect on diffusion in nanoscale was also investigated.

This is the second in a series of articles demonstrating the unique character of the aerosol-through-plasma (A-T-P) process for producing nanoparticles. This study is focused on the impact of two parameters, cation ratio (1:3, 1:1, 3:1) and solvent (evaporated prior to generation of aerosol), on the structures of Ce:Al oxides particles. These two simple changes were found to impact virtually every aspect of particle structure, including the fraction of hollow versus solid, fraction of nanoparticles, phase structure, and even the existence of surface phase segregation. CeAl mixed oxides were found only over a limited range of compositions, and that range was a function of the solvent. At all other cation ratios, only ceria was a crystalline phase, and most if not all the alumina is amorphous. It is notable that the fraction of hollow micron-sized particles and nanoparticles is greatly influenced by the cation ratio and solvent identity. Indeed, significant numbers of nanoparticles were only produced using an aqueous precursor with a Ce:Al ratio of 1:1. Another unique finding is that phase segregation exists in individual particles on the length scale of nanometers. This study compliments an earlier study of the influence of operating conditions on particle structure. Taken together, the studies suggest a means to engineer (as well as limits to the engineering possibilities) ceramic particle structures using the A-T-P method.

The electrochemical and corrosion behaviors of solder alloys—SnAgCu (SAC), SnZnBi, SnPb, and Sn—and printed circuit board finish materials Cu and AuNi were investigated in carboxylic acids (flux) and NaCl solutions using the potentiodynamic scanning technique. The results show that SAC and Sn are passivated in the diluted flux solution, but SnPb, SnZnBi, Cu, and AuNi are under active dissolution when anodically polarized. However, passivation of SAC alloy is not observed in concentrated flux solution. Although a passive film forms on SAC in a 2% NaCl solution, the film is less stable than in the flux solution. In addition, oxidation of the most commonly used lead-free and lead solders, SAC and SnPb, at high temperature was evaluated via sequential electrochemical reduction analysis (SERA). The SERA results revealed that the SAC alloy oxidized more significantly than SnPb under hot, dry conditions.

The effect of changes in poly(acrylic acid) (PAA) conformation on removal of Si3N4 film was investigated. PAA was used as a passivation agent by adsorption on an Si3N4 film in shallow-trench isolation chemical–mechanical planarization (STI CMP). Adsorption behavior of PAA on the Si3N4 film and the conformation transition were determined by adsorption isotherms and force measurements using atomic force microscopy (AFM) as a function of ionic strength. AFM results revealed that, as ionic strength increases, the repulsive force between the negatively charged carboxylate groups along the backbone of PAA is reduced due to counterion screening and to the changes of PAA conformation from a stretched to a coiled configuration. At high ionic strength, the coiled conformation of PAA formed a dense passivation layer on the Si3N4 film, which led to suppression of the removal rate of Si3N4 film from 72 to 61 Å/min in the STI CMP process.

MgTe2O5 ceramics were prepared by solid-state route. These materials were sintered in the temperature range of 640–720 °C. The structure and microstructure of the compound was investigated using x-ray diffraction (XRD), Fourier transform infrared (FTIR), Raman spectroscopy, and scanning electron microscopy (SEM) techniques. The dielectric properties of the ceramics were studied in the frequency range 4–6 GHz. The MgTe2O5 ceramics have a dielectric constant (ϵr) of 10.5, quality factors (Qu × f) of 61000 at 5.3 GHz, and temperature coefficient of resonant frequency (τf) of −45 ppm/°C at the optimized sintering temperature of 700 °C. The microwave dielectric properties of these materials at cryogenic temperatures were also investigated.