Detailed understanding of growth termination in vertically aligned single-walled carbon nanotubes (SWNTs) made via supergrowth, or water-assisted growth, remains critical to achieving the ultralong SWNTs necessary for next-generation applications. We describe the irreversible catalyst morphology evolution that occurs during growth, and which limits the lifetime of surface supported catalysts. Growth termination is strongly dependent on growth temperature, but not sensitive to C2H2:H2O ratio. In addition to both planar Ostwald ripening of small (sub-5 nm) Fe catalyst particles and diffusion of metal atoms into the alumina support, other features that contribute to growth termination or deceleration are described, including center-of-mass particle motions and coalescence of smaller species of surface supported Fe nanoparticles. Additionally, a temperature-induced structural transition in the alumina catalyst support is found to be coincident with abrupt growth termination at temperatures of 800 °C and higher. In situ electron microscopy observations are used to directly support these observations.

Thin films of c-axis-oriented LiCoO2 were epitaxially grown by pulsed laser deposition (PLD). The ablation laser conditions greatly affect the crystal quality of the epitaxial LiCoO2 thin films. In addition, high-quality LiCoO2 thin films were found to grow without any impurity phases under relatively low oxygen partial pressure, although high pressure had been often selected to suppress the formation of Co3O4 with a lower valence state as an impurity. This result clearly indicates that the ablation laser conditions are an essential growth parameter, and that composition control is indispensable to grow high-quality complex compound thin films by PLD.

Synchrotron x-ray μ-tomography has been used to reconstruct the three-dimensional view of a rough surface extracted from a heterogeneous ceramic coating composed of Pr2NiO4+δ. Radiographs with a resolution of 0.7 μm have been recorded at T = 300, 600, and 900 K. The analysis of surface geometry makes use of the geometrical optic approximation up to T = 900 K possible. Subsequently, a large number of rays (105) are impinged onto the numerical surface, as revealed by x-ray tomography, to reproduce the normal emissivity of the coating. This normal emissivity was obtained beforehand by infrared emittance spectroscopy at T = 1000 K. Comparison of the two approaches suggests that the optical contribution of the coating micropores can be integrated into the ray tracing code. The effective medium approximation is used for this purpose. Finally, the applicability of this hybrid approach is discussed.

The physical and electrical properties of La2O3 with and without an Al2O3 capping layer deposited by remote plasma atomic layer deposition were investigated. The electrical properties of the La2O3 films degraded due to the formation of lanthanum hydroxide after being exposed to air. The results of x-ray photoemission spectroscopy showed that the quantity of OH groups absorbed increased after exposure to air. For La2O3 with an Al2O3 capping layer, however, the electrical properties of the film did not change substantially because the capping layer effectively suppressed the formation of lanthanum hydroxide. The capacitance of the La2O3 decreased more than 30% after exposure to air, while La2O3 with an Al2O3 capping layer decreased by only about 4%. The VFB value of the La2O3 with an Al2O3 capping layer was near zero, and the hysteresis was about 120 mV. The leakage current densities of the film were maintained below 5 × 10−7 A/cm2 up to −15 MV/cm and the effective breakdown field was about −23.5 MV/cm.

We describe progress in understanding the effect of simulated chemical-mechanical planarization (CMP) slurry chemistry on the evolution of defects and formation of damage that occurs during CMP processing. Specifically, we demonstrate the significant effect of aqueous solution chemistry on accelerating crack growth in porous methylsilsesquioxane (MSSQ) films. In addition, we show that the same aqueous solutions can diffuse rapidly into the highly hydrophobic nanoporous MSSQ films containing interconnected porosity. Such diffusion has deleterious effects on both dielectric properties and the acceleration of defect growth rates. Crack propagation rates were measured in several CMP solutions, and the resulting crack growth behavior was used to qualitatively predict the extent of damage during CMP. These predictions are compared with damage formed during actual CMP processes in identical chemistries. We discuss the effects of both the high and low crack growth rate regimes, including the presence of a crack growth threshold, on the predicted CMP damage. Finally, implications for improved CMP processing were considered.

An experimental study on the adhesion of thin films was conducted for the ultraviolet (UV)-cured SiOC films on Si substrate by examining the mechanical energy balance during the indentation process combined with atomic force microscopy observation. The effect of UV cure on the interfacial delamination toughness and the structure of the SiOC films are discussed. The energy release rate of the SiOC film/Si substrate interfacial delamination increases with the increases in the time of UV curing, indicating that the indentation method is efficient to examine the adhesion of coating. As the UV curing time increases, the film thickness and the Si–CH3 bond structure decrease, whereas the SiO2 network structure develops and the mechanical properties of the film are improved. Furthermore, the energy release rate of SiOC film/Si interfacial delamination is well correlated in a proportional manner to the Young's modulus of the film.

We developed a new microscale technique for evaluating the local interface adhesion in a thin film stack and we compared it with a conventional four-point bending technique. Using the microscale technique, the interface adhesion was estimated to be 3.0 J/m2 by comparing experimental results with numerical simulation results for interface crack propagation behavior. The four-point bending technique was applied to the same interface and the interface adhesion was estimated to be 4.4 J/m2 by experiment. However, this value is an overestimate because it includes the plastic deformation of epoxy resin used to fabricate the specimens. By eliminating the additional energy dissipated through plastic deformation of the epoxy resin close to the interface crack tip, the interface adhesion was evaluated to be 3.3 J/m2. This value agrees well with that obtained using the microscale technique.

Low energy metal ion implantation has been used to combine an easy “bottom-up” way of creating and tuning different topographic structures on submicron to micrometer scales with the embedding of a metallic element-rich functionalized layer at the surface for a variety of scientific and technological applications. The self-organizing and complex patterns of functionalized topographic structures are highly dependent on the implanted metal ion species, variations in the geometric confinement of the buckled areas on the larger unmodified elastomer film, and the boundary conditions of the buckled regions. Systematic investigations of these dependencies have been carried out via optical and atomic force microscopy, and confirmed with cross-sectional transmission electron microscopy.

An effective way to prepare a robust CuInSe2 (CIS) target for subsequent vapor depositions of thin films is suggested in this work. The technique involves addition of excess Se to presynthesized CIS powder followed by cold pressing and sintering at a temperature as low as 300 °C. Phase-pure chalcopyrite CIS films were prepared at a substrate temperature of 300 °C from targets that contained different amounts of excess Se. The average size of particulates, typical of the pulsed laser deposition process, and their surface coverage decreased with increasing Se content up to 50 wt% in the targets. Films grown from the target with 50 wt% excess Se exhibited a hole concentration of ˜3 × 1019 cm−3 and a Hall mobility of ˜2 cm2/Vs. With the decrease of substrate temperature to room temperature, the resistivity increased from 1.1 × 10−1 to ˜7.5 × 108 Ω·cm, which is attributed to the potential contributions of Se interstitials, CuIn, and VIn defects.

A new Pd79Au1.5Ag3Si16.5 bulk metallic glass was successfully synthesized in a maximum casting thickness range to 3 mm. Upon heating, the single glassy phase decomposed into Pd-rich crystalline phases and a Si-rich amorphous phase due to solute partitioning. In addition to high thermal stability, this bulk glassy alloy also exhibited a high degree of ductility and excellent corrosion resistance, showing potential applications as biomaterials.

Electron backscatter diffraction analysis was used to compare the crystal orientation of β-Sn grains in Ni(P)/Sn–0.5Cu/Cu and Ni(P)/Sn–1.8Ag/Cu joints before and after aging. In Ni(P)/solder/Cu joints, the solder composition (Cu versus Ag) significantly affects β-Sn grain orientation. In Ni(P)/Sn–0.5Cu/Cu, there are two types of small columnar grains grown from Ni(P) and Cu under bump metallurgy with a high-angle grain boundary crossing the joint closer to the Ni side; in contrast, Ni(P)/Sn–1.8Ag/Cu has large grains with low-angle boundaries. During thermal aging at 150 °C for 250 h, the Ni(P)/Sn–0.5Cu/Cu joints undergo a more significant microstructural change than the Ni(P)/Sn–1.8Ag/Cu joint. Additionally, obvious ledges developed along the high-angle grain boundary between the upper and lower areas in the Sn–0.5Cu joint.

It has been shown that the stability of shear banding and plasticity of bulk metallic glasses (BMGs) can be strongly influenced by the machine stiffness. Here, we demonstrated that the practice of adding a frame parallel to the sample is quantitatively equivalent to increasing the machine stiffness by the frame stiffness. A series of carefully designed experiments were conducted to verify such an effect, showing controllably enhanced plasticity of BMG samples.

Applying glass fluxing and cyclic superheating, rapid solidification of undercooled Ni–15at.%Cu alloy was performed by rapidly quenching the sample after recalescence. The evolution of microstructure and microtexture has been analyzed. At both low and high undercoolings, well-developed dendrites, within and around which are distributed by the fine equiaxed grains, are observed. At low undercooling, the completely grain-refined microstructure shows a highly oriented texture without annealing twins, whereas at high undercooling a fully random texture as well as a number of annealing twins is observed. On this basis, all the possible mechanisms for grain refinement, as well as their effects on the microstructure formation, were discussed. The grain refinement at both low and high undercoolings is concluded to originate from dendrite fragmentation. Particularly, at high undercooling, recrystallization, as a consequence of dendrite deformation (by fluid flow) and dendrite fragmentation (which provides grain boundary sites for recrystallization nucleation and for the “appearing” recrystallized grains), occurs and plays a role in the grain refinement and the formation of fully random texture.

The tensile deformation of anisotropic porous copper with unidirectionally oriented cylindrical pores was investigated by an acoustic emission method. In the loadings parallel and perpendicular to the orientation direction of the pores, many cracks are formed after yielding and they strongly affect the deformation. The formed cracks rapidly grow and connect with each other near the peak stress of the stress–strain curve, thereby leading to final fracture. Crack formation is easier under perpendicular loading than under parallel loading, because high stress concentration and stress triaxiality occurs around the pores. As a result, the strength and elongation for perpendicular loading are much smaller than those for parallel loading. Furthermore, in the case of perpendicular loading, the localized deformation around pores drastically decreases the plastic Poisson's ratio. These results indicate that a porous copper macroscopically behaves as a semibrittle material under perpendicular loading, while the porous copper exhibits ductility under parallel loading.

Images of synchro-Shockley partial dislocation arrangements in the Laves phases NbCr2 and HfCr2 have been obtained by high-resolution transmission electron microscopy. The analysis of the stacking sequences around these arrangements revealed the role of the constituting partial dislocations in enabling the polytypic C14 → C36/6H phase transformation in both alloys. The synchro-Shockley partial dislocations occur in and move through the crystals mainly as dipoles of partials of opposite signs, leading to—as compared to isolated partials—strain fields of lesser extent. In NbCr2 a single, probably quenched synchro-Shockley partial dislocation dipole, consisting of two partials with Burgers vectors of opposite sign, was identified. The ordered passage of a series of this type of line defects brings about the C14 → C36 transformation. In HfCr2 a complex synchro-Shockley partial dislocation configuration was revealed. It can be regarded as an “antiphase boundary” between two C36 domains. It is likely that this defect structure had formed by impingement of two domains of C36 growing perpendicular to the stacking direction by glide of synchro-Shockley partial dislocation dipoles.

Hierarchical and hollow SnS2 nanostructures as precursors were fabricated via a surfactant-assisted assembly process using sodium dodecyl sulfate as soft templates. The as-prepared SnS2 nanostructures were further oxidized to form porous SnO2 conversion for investigating their gas-sensing properties in drug-precursor detection. On the basis of a series of time- and ratio-dependent reactions, a formation mechanism of the special nanostructures and factors influencing morphology and structure were determined. Gas-sensing measurements revealed that the porous and hierarchical SnO2 hollow nanostructures were sensitive to drug precursors, indicating promising applications in environmental monitoring and public safety investigation. In addition, we found that the assembled SnO2 nanomaterials possessed significantly enhanced gas-sensing properties compared with unassembled SnO2 with a solid interior.

We fabricated a nanostructured brush by carrying out Ni deposition on a through-channel anodic aluminum oxide (AAO) template, followed by removal of the AAO skeleton. The AAO was prepared by a two-step anodization process resulting in pore diameter and thickness of 350 nm and 40 μm, respectively. Subsequently, the AAO underwent an electroless deposition involving sensitization, activation, and Ni plating, in conjunction with polyethylene glycol used as the inhibitor to prevent premature closing of pore opening. After deliberate control in relevant parameters, we obtained a conformal Ni overcoat along every pore channel leading to a reduced average pore diameter of 78 nm. Afterward, the sample was immersed in a KOH solution to remove the AAO structure, forming freestanding Ni tubules in a brush configuration. The nanostructured brush revealed considerable enhancement for hydrogen evolution reaction in both current-potential polarization and galvanostatic measurements, which were attributed to the increment in apparent surface area.

The reversible hydrogen adsorption site in Ni-nanoparticle-dispersed amorphous silica (Si-O) was identified by analyzing the hydrogen adsorption behavior and the microstructure. The total amount of reversibly adsorbed hydrogen was evaluated from the total surface area of Ni and the Ni concentration in the composite. The total surface area of the Ni nanoparticles in each sample powder was calculated from the mean particle size of the Ni nanoparticles in the Si-O matrix using dark field images taken by transmission electron microscopy and high-angle annular dark-field images by scanning transmission electron microscopy. The estimated amount of reversibly adsorbed hydrogen was highly consistent with that obtained experimentally by hydrogen adsorption analysis, which suggested that reversible hydrogen adsorption occurred at the Ni/Si-O interface.

Niobium and tantalum doped anatase were prepared by thermal hydrolysis of peroxotitanium complex aqueous solutions containing of niobium or tantalum peroxo-complexes at 100 °C for 3 days. Niobium-doping increased the unit cell constants of anatase and changed the morphology of TiO2 from spindle-like to rectangular or square cross section. Nb and Ta doping in the TiO2 nanostructure increases the anatase to rutile transformation temperature to >1000 °C. In the visible region, the photocatalytic activity is directly proportional to the concentration and increases with increasing of Nb concentration. The niobium addition enhances the photocatalytic activity of titania in the visible light region.

Ultra fine CuO nanoparticles in the range of 2 ± 0.2 nm were synthesized by the supercritical hydrothermal method in a batch reactor. It was demonstrated that elevating the pH of the Cu2+ precursor solution to around 6 (neutral condition) not only does not lead to excessive agglomeration of the particles, but also reduces particle size and in general promotes their nanoscale characteristics. Prepared nanoparticles were immobilized in the biopolymeric matrix of barium alginate and calcined at different temperatures resulting in microspherical granules of high porosity and elevated mechanical strength. The fabricated samples were characterized using x-ray diffractometry (XRD), transmission and scanning electron microscopy (TEM and SEM), nitrogen adsorption analysis (BET), mechanical testing, and temperature programmed reduction (TPR). It was found that topochemical models based on a nucleation growth mechanism fail in proper fitting of the TPR data. Instead, a generalized Sestak model in which different physicochemical mechanisms such as the mass action law are taken into account gives a satisfactory regression of the kinetics behavior.