Finite element analysis is used to simulate cone indentation creep in materials across a wide range of hardness, strain rate sensitivity, and work-hardening exponent. Modeling reveals that the commonly held assumption of the hardness strain rate sensitivity (mH) equaling the flow stress strain rate sensitivity (mσ) is violated except in low hardness/modulus materials. Another commonly held assumption is that for self-similar indenters the indent area increases in proportion to the (depth)2 during creep. This assumption is also violated. Both violations are readily explained by noting that the proportionality “constants” relating (i) hardness to flow stress and (ii) area to (depth)2 are, in reality, functions of hardness/modulus ratio, which changes during creep. Experiments on silicon, fused silica, bulk metallic glass, and poly methyl methacrylate verify the breakdown of the area-(depth)2 relation, consistent with the theory. A method is provided for estimating area from depth during creep.

Glancing-incidence x-ray diffraction (GIXRD) has been applied to the investigation of depth-dependent stress distributions within electroplated Cu films due to overlying capping layers. Cu films, 0.65 μm thick, plated on conventional barrier and seed layers received a chemical vapor deposited (CVD) SiCxNyHz cap, an electrolessly deposited CoWP layer, or a CoWP layer followed by a SiCxNyHz cap. GIXRD and conventional x-ray diffraction measurements revealed that strain gradients were created in Cu films possessing a SiCxNyHz cap, where a greater in-plane tensile stress of approximately 180 MPa was generated near the film/cap interface as a result of constraint imposed by the SiCxNyHz layer during cooling from the cap deposition temperature. Although Cu films possessing a CoWP cap without a SiCxNyHz layer did not exhibit depth-dependent stress distributions, subsequent annealing introduced stress gradients and increased the bulk Cu stress. However, a thermal excursion to liquid-nitrogen temperatures significantly reduced tensile stresses in the Cu films.

Using nanoindentation, this study develops the criteria to evaluate the creep performance of the intermetallic compounds (IMCs) formed at the interface of microelectronic solder joints. Regardless of crystal structure and melting point, the creep stress exponent (X), one of the parameters determining creep resistance, is in good agreement with tendencies of the work-hardening exponent (n) and also the ratio of yield stress (Y) to Young's modulus (E), which reveals the ability against plastic deformation.

A new physical method is described for the preparation of metal microspheres by ultrasonic cavitation of low-melting point metals (<380 °C) immersed in hot silicone oil. The ultrasonic radiation causes dispersion of the molten metals into spheres, which solidify rapidly on cooling. This method is illustrated for the synthesis of Pb and Au–Si eutectic alloy.

Phase-pure nanostructured WB ceramics are hot pressed at ultrahigh pressures of 1.0 to 3.0 GPa and high temperatures of 700 to 1000 °C (UHPHT) for 60 min. The UHPHT samples are nanograin size from 15 to 40 nm. Our experimental observation shows that ultrahigh pressure could improve densification, and the density of WB samples could reach 99.4% of theoretical. The comparative experiments carried out at ambient pressure and temperatures of 550 to 1100 °C for 60 min indicate that the external pressure was favorable for phase-pure and highly dense WB formation. In addition, the UHPHT samples give a high hardness value of 28.9 ± 0.8 GPa.

This paper presents experimental and theoretical studies of the adhesion between the drug-eluting layer and a Parylene C primer layer in coatings present on a model drug-eluting stent. To quantify adhesion, Brazil nut sandwich specimens were prepared mimicking the layers of this coating. These samples were stressed to fracture, and the resulting initial cracks at the Parylene C/drug interface were used to measure the dependence of interfacial fracture energy of mode mixity. The mating fracture surfaces were then analyzed using scanning electron microscopy (SEM) and energy dispersive x-ray spectroscopy (EDX). The interfacial energy release rates were obtained over a wide variety of mode mixities. Adhesion and fracture mechanics models were then used to estimate the mode mixity dependency of interfacial fracture toughness. Fracture toughness was found to be larger under higher mode mixity than that under lower mixity and the analytical model showed close agreement with experimental results.

The cooperative self-assembly of organic–inorganic siliceous composite structures has been studied from the aspect of inorganic precursors. We reveal that the vesicular or mesostructured materials can be obtained selectively by just changing the silica sources in one templating system. For poly(ethylene oxide)-type block copolymers with either poly(propylene oxide) or poly(butylene oxide) as the hydrophobic moieties, when the other synthesis parameters are exactly the same, the use of tetramethyl orthosilicate (TMOS) as a silica source gives rise to highly ordered mesostructures, while the use of tetraethyl orthosilicate (TEOS) leads to vesicles or foams. The attenuated total reflection Fourier transform infrared (ATR-FTIR) technique is used to monitor the silicate species derived from the hydrolysis and condensation of TMOS and TEOS as a function of the reaction time. On the basis of the ATR-FTIR results, we propose a “differentiating effect” at relatively high pH (4.7) to interpret the influence of different silica sources on the self-organized composite structures. For comparison, a “leveling effect” at relatively low pH (strong acidic conditions) is revealed to explain that both TMOS and TEOS lead to the same mesostructures. Our contribution provides a feasible and designable method to synthesize from conventional ordered mesostructures to novel vesicular structures, which are significant for their future practical applications.

Layer-structured polypyrrole/montmorillonite (PPy/MMT) naoncomposite films were synthesized by the electrodeposition method. The fabricated free-standing films consist of about 0∼2 wt% Na+-montmorillonite (NMMT). The thickness of films could be controlled by deposition time. X-ray diffraction (XRD) and scanning electron microscope (SEM) were used to observe the microstructure of the films. After MMT was introduced into the PPy matrix, the interspace between PPy chains decreased, according to the XRD results. The layered structure of the films was observed from the SEM images. Tensile and nanoindentation test results showed that the mechanical properties of the composite films were improved at low clay loading. The electrical conductivity of the films with 1.2 wt% MMT loading was increased from 3.6 to 51 S/cm, probably because of the restricted growth of PPy chains in the interspace of MMT layers.

YB22C2N is one of a series of rare earth borocarbonitrides and is potentially the long awaited n-type counterpart to boron carbide. We conducted studies on YB22C2N spark plasma sintered with additions of YB4 and YB25C, including the investigations of the densification process and the thermoelectric properties of the material. We discovered that a small amount of dopants can lower the starting temperature of densification during spark plasma sintering (SPS). Variations of pressure and temperature during the sintering process are also found to have an effect. Electrical conductivity of the dense samples has increased due to insertion of metal borides and also because of the improvement of the relative density. At the same time, only a slight reduction was observed for the Seebeck coefficient leading to an important improvement of power factor. The highest density of more than 95% was achieved with 5 wt% of YB25(C) dopant.

The authors report a study of molecular beam deposition of MgO films on amorphous SiO2 and (0001) GaN surfaces over a large range of temperatures (25–400 °C) and molecular oxygen growth pressures (10−7–10−4 Torr). This study provides insight into the growth behavior of an oxide with volatile metal constituents. Unlike other materials containing volatile constituents (e.g., GaAs, PbTiO3), all components of MgO become volatile at normal epitaxial growth temperatures (≥250 °C). Consequently, defining which species is the adsorption controller becomes ambiguous. Different growth regimes are delineated by the critical substrate temperature for Mg re-evaporation and the Mg:O flux ratio. These regimes have impact on phase purity, quartz crystal microbalance calibration, and film microstructure. The universal decay in deposition rate above growth 10−5 Torr O2 is also considered. By introducing a third flux of inert argon gas, rate reduction is attributed to increased molecular scattering and not oxidation of the metal source.

The structure and properties of HfO2 films deposited by plasma assisted reactive pulsed laser deposition and annealed in N2 were studied upon thermal annealing as well as the evaluation of thermal stability by Fourier transform infrared spectroscopy, spectroscopic ellipsometry, and optical transmission measurements. The as-deposited HfO2 films appear predominantly monoclinic with an amorphous matrix which becomes crystallized after high-temperature annealing. No interfacial SiOx is observed for the as-deposited films on Si. The deposited HfO2 films exhibit good thermal stability and show excellent transparency in a wide spectral range with optical band gap energies of 5.65–5.73 eV depending on annealing temperature. An improvement in the optical properties by high-temperature annealing is also observed.

This paper demonstrates the production of 〈00l〉-oriented CuO-doped (K0.476Na0.524)NbO3 (KNN) piezoelectric ceramics with a polymorphic phase transition (PPT) temperature greater than 180 °C by templated grain growth (TGG) using high aspect ratio NaNbO3 template particles. A novel (to the KNN system) two-step sintering and annealing process combined with CuO doping is demonstrated to improve density and maximize texture quality (F00l = 99% and rocking curve FWHM = 6.9°) in textured KNN ceramics. The best electromechanical properties (kp ≈ 0.58, k31 ≈ 0.33, d33 ≈ 146 pC/N, To-t ≈ 183 °C, Tc ≈ 415 °C, εr = 202, and tan δ = 0.016) are achieved in 1 mol% CuO-doped KNN with F00l = 99% and a relative density of 96.3%. The values of d33, kp, and k31 are 70–90% higher than randomly oriented ceramics and are obtained without a significant reduction in the PPT temperature, resulting in stable piezoelectric performance over a wide temperature range (−50 to 180 °C). These results show that high-quality textured KNN can be obtained by TGG and that a reactive matrix is unnecessary.

Thin-film transistors (TFTs) with zinc oxide channel layers were fabricated through a simple and low-cost solution process. Precursor solution concentration, annealing temperature, and the process were controlled for the purpose of improving the electrical properties of ZnO TFTs and analyzed in terms of microstructural scope. The fabricated ZnO films show preferential orientation of the (002) plane, which contributes to enhanced electron conduction and a dense surface. The results show that the TFT characteristics of the film are clearly affected by the microstructure. The optimized TFT operates in a depletion mode, shows n-type semiconductor behavior, and is highly transparent (>90%) within the visible light range. It exhibits a channel mobility of 9.4 cm2/V·s, a subthreshold slope of 3.3 V/decade, and an on-to-off current ratio greater than 105. In addition, the result of N2 annealing shows the possibility of improvement in electrical property of the ZnO TFTs.

To fabricate graded-index optical elements by silver staining, we investigated the behavior of ion incorporation in aluminoborosilicate glasses, in which the contents of Al2O3 and Na2O were the same (in mol%). The amount of silver incorporated into the aluminoborosilicate glasses by the staining at 320 °C for 12 h was 5 to 10 times larger than that incorporated into the soda-lime silicate and borosilicate glasses. The diffusion depth of the incorporated silver ions was approximately 80 μm, which was also much deeper than that of the soda-lime silicate and borosilicate glasses. The coloration of the glasses was suppressed, particularly for the glass with the low content of Na2O. The concentration of the incorporated silver ions at the glass surface was 2 × 1021 atom/cm3 for the 37.5SiO2·25Al2O3·25Na2O·12.5B2O3 glass, corresponding to the replacement of sodium ions (20%). The refractive indices near the stained surfaces increased by 0.04 to 0.06. These values were comparable with those of the soda-lime silicate and borosilicate glasses.

4H-silicon carbide (SiC) wafers were annealed at 1300 and 1600 °C for 30 min and 60 min in a conventional and purified Ar atmosphere. The surface roughness before and after annealing was evaluated by atomic force microscopy. The surface roughness before annealing was approximately 2.37 nm in root mean square. The roughness, after annealing for 30 min at 1300 and 1600 °C in a conventional Ar furnace, was increased to 4.53 and 14.9 nm, respectively. The roughness, after annealing for 60 min, was 5.01 and 19.1 nm, respectively. In this study, the G3 grade Ar gas (99.999%) was supplied in the conventional furnace tube. When the Ar gas was purified to an impurity concentration of less than 1 ppb, and it was supplied in the leak-tight furnace tube, the roughness after 30-min annealing improved 4.27 and 6.93 nm at 1300 and 1600 °C, respectively. The roughness after 60-min annealing was also reduced to 3.54 and 9.28 nm, respectively. We assume that a significant reduction of H2O concentration in the annealing atmosphere might play an important role in suppressing surface roughening of SiC during high-temperature annealing.

PtPd@Pt core-shell ultrathin nanowires were prepared using a one-step phase-transfer approach. The diameters of the nanowires range from 2 to 3 nm, and their lengths are up to hundreds of nanometers. Line scanning electron energy loss spectra showed that PtPd bimetallic nanowires have a core-shell structure, with a PtPd alloy core and a Pt monolayer shell. X-ray absorption near edge structure (XANES) spectra reveal that a strong Pt-Pd interaction exists in this nanowire system in that there is PtPd alloying and/or interfacial interaction. Extended x-ray absorption fine structures (EXAFS) further confirms the PtPd@Pt core-shell structure. The bimetallic nanowires were determined to be face-centered cubic structures. The long-chain organic molecules of n-dodecyl trimethylammonium bromide and octadecylamine, used as surfactants during synthesis, were clearly observed using aberration-corrected TEM operated at 80 KV. The interaction of Pt and surfactants was also revealed by EXAFS.

Several binary intermetallic compounds—each containing a rare-earth (RE) element paired with a transition metal (TM)—were prepared by self-propagating, high-temperature synthesis (SHS). Thin multilayers, composed of alternating Sc or Y (RE element) and Ag, Cu, or Au (TM), were first deposited by direct current magnetron sputtering. Once the initially distinct layers were stimulated and caused to mix, exothermic reactions propagated to completion. X-ray diffraction revealed that Sc/Au, Sc/Cu, Y/Au, and Y/Cu multilayers react in vacuum to form single-phase, cubic B2 structures. Multilayers containing Ag and a RE metal formed cubic B2 (RE)Ag and a minority (RE)Ag2 phase. The influence of an oxygen-containing environment on the reaction dynamics and the formation of phase were investigated, providing evidence for the participation of secondary combustion reactions during metal-metal SHS. High-speed photography demonstrated reaction propagation speeds that ranged from 0.1–40.0 m/s (dependent on material system and foil design). Both steady and spin-like reaction modes were observed.

Indentation experiments on thin films are analyzed by using a rigorous solution to model elastic substrate effects. Two cases are discussed: elastic indentations where film and substrate are anisotropic and elastoplastic indentations where significant material pileup occurs. We demonstrate that the elastic modulus of a thin film can be accurately measured in both cases, even if there is significant elastic mismatch between film and substrate.

A new function that describes the shape of three-sided pyramidal indenters is introduced. This function differs from the polynomial tip shape function conventionally used in nanoindentation tip shape calibration in that the new function includes fewer fitting parameters with clearer physical meaning. Specifically, two of the fitting parameters integrated into the new function are the indenter’s tip radius and the slope of the indenter’s equivalent cone. Tip shape calibration data were collected with four different diamond indenter tips, and both the new function and the standard polynomial function were fit to the data. It is found that the new function can fit calibration data nearly as well as the standard polynomial function and better than existing physically based functions. Although the tip radius parameter obtained by fitting the new model to data deviates from the tip radius determined from Hertzian elastic contact, the two values are correlated.

The very high strengths that have been reported for nanoporous gold may be related to strain gradients within the deforming porous microstructure. We present a mechanism-based model for the strength of nanoporous foams that is derived from conventional models for the deformation of macroscopic foams and now includes the influence of strain gradients. This model predicts that the strength of the ligaments within the nanoporous gold is proportional to the ligament diameter raised to the power −0.5. We have used the model to analyze experimental data for the strength of nanoporous gold and find excellent agreement with published data.