A neural network-based analysis method for the identification of a viscoplasticity model from spherical indentation data, developed in the first part of this work [J. Mater. Res.21, 664 (2006)], was applied for different metallic materials. Besides the comparison of typical parameters like Young’s modulus and yield stress with values from tensile experiments, the uncertainties in the identified material parameters representing modulus, hardening behavior, and viscosity were investigated in relation to different sources. Variations in the indentation position, tip radius, force application rate, and surface preparation were considered. The extensive experimental validation showed that the applied neural networks are very robust and show small variation coefficients, especially regarding the important parameters of Young’s modulus and yield stress. On the other hand, important requirements were quantified, which included a very good spherical indenter geometry and good surface preparation to obtain reliable results.

Over millions of years, natural constructions have been developed by evolutionary processes in nature with the general aim to generate high-performance structures with minimum material consumption. It is well known that one of the major strategies is to reach a largely homogeneous material load in the biological structure. In this paper, we demonstrate that this natural design principal applies not only to the macroscopic level but also to microstructural optimization, and in particular, to adhesive joints in nature. Furthermore, we introduce the computer aided adhesive and assembly optimization method (CA3O), which transfers the natural mechanically stimulated growth processes to technical adhesive joints by means of the finite element method.

Pr-doped ZnO phosphor powders were prepared by dry reaction within evacuated sealed silica glass tube. Pr2O3 and Pr6O11 were used as additives. Pr concentrations were 0.5, 1, 3, and 5 mol%, and the sintering temperatures were 600, 800, and 1000 °C, respectively. Photoluminescence (PL) and PL excitation (PLE) spectra were measured to study luminescent properties of samples. Some samples showed the enhancement of green emission. This emission is related to native defects in ZnO. Based on the results of PL and PLE, the origin of the enhancement was discussed in view of native defects in ZnO and the defect-related complex in ZnO varistor ceramics. The possible origin is the increase of native defects such as VZn, OZn, and the complex in the vicinity of grain boundaries and ZnO matrix near the surface of grains. The increase of native defects and the complex are probably due to the existence of the Pr3+-ions with binding to native defects, which form the complex by Coulombic potential.

Repeated deformation processing was used to produce layered aluminium titanate (ATI)-alumina composites with a corrugated microstructure. Viscous nonpolar pastes of ATI and alumina powders were prepared using paraffin oil as the dispersing medium. These pastes were rolled into tapes 1 mm thick, which were then stacked together to form starting bi-material laminates in an A-B-A sequence. The laminates were then plastically deformed by repeated folding and rolling at room temperature. After a sufficiently large true plastic deformation, composites with corrugated microstructures were successfully produced. During sintering, part of the ATI decomposed; in the alumina layers large anisotropic grains were formed. The mechanical properties of the sintered composites improved with structural refinement, in spite of extensive microcracking observed during cooling from the sintering temperature. In addition, the thermal expansion coefficient along the rolling direction did not differ from that of the reference material.

Structural characterization at the nanometric scale of the Nautilus sp shell was carried out by high-resolution transmission electron microscopy and high-angle annular dark field to understand how the organic and inorganic components are related. The inorganic phase that built the shell is made of calcium carbonate (CaCO3), with the orthorhombic unit cell of the aragonite, in a texturized arrangement in such a way that the c-axis is always perpendicular to the shell surface. The organic material forms films through the plates. We observed for a very first time some aragonite nanocrystals embedded in the organic matrix. This observation supports the hypothesis that the proteins and other organic compounds guide the crystal growth because the organic matrixes are the places where the nanocrystals grow.

The local deformation surrounding an indented area of Ensis siliqua mollusk shell is characterized using a Raman spectroscopic technique, the findings of which are related to the material’s mechanical function. Microhardness indentation of four directional planes is used to show the marked anisotropy of the structure, where the outer and inner layers of the shell are found to have a significantly higher microhardness value of 4.82 ± 0.02 GPa, compared with transverse and longitudinal cross-sectional values of 3.00 ± 0.07 GPa. This difference is related to the crossed lamellar microstructure of the shell, which is oriented to provide the maximum resistance to external attack from predators. Nanoindentation of the material shows no such anisotropy, giving mean hardness and modulus values for the four directional planes of 3.86 ± 0.10 GPa and 82.4 ± 2.7 GPa respectively, thereby clarifying the prominent role of microstructure in such materials. Scanning electron microscopy of indented samples shows that plastic deformation and delamination occur to different extents, depending on the orientation of the structure and local microstructural features such as prismatic layers. A Raman spectroscopic technique has been used to map relative deformation in the vicinity of the indents, showing that the amount of plastic or permanent deformation can be quantified, and that material delamination can be distinguished from other forms of deformation such as local cracking. These experimental methods are repeated using samples of non-biogenic aragonite, which act as an analogous material for comparison with the shell. It is proposed that the analysis of microhardness indents using Raman spectroscopy could be applied to other biomaterials exhibiting anisotropy.

Size-tuned ZnO nanorod arrays (NRAs), aligned well vertically and laterally, were synthesized by catalyst-free, metalorganic chemical vapor deposition on GaN-buffered Al2O3 (0001) substrates by adjusting the O/Zn precursor ratio in the reactor. Their electrical transport properties were investigated using field effect transistors based on individual ZnO nanorods. We find that the carrier concentrations and mobilities in the nanorods are not very sensitive to the change of the precursor ratio. This suggests that altering the precursor ratio is a way of fabricating size-tuned ZnO NRAs with quite consistent electrical properties.

Effects of particle size of Cr2O3 catalyst on the hydrogen absorption/desorption kinetics of Mg + 5 wt% Cr2O3 mixtures have been studied. To explain the effect of particle size of Cr2O3 and also to yield information about the role of Cr2O3 during the sorption process, the kinetics data have been analyzed using Avrami–Erofeev rate equations. The activation energies and diffusion coefficients of these mixtures are in the ranges of 50.6–63.2 kJ/mol and 1.2.10−11 to 8.9.10−10 cm2/s, respectively. The addition of nano-oxides led to an increase of the diffusion coefficient of hydrogen by one order of magnitude.

Multilayered Co/Cu nanowires were fabricated using anodic alumina templates, containing 40-nm-diameter nanopores, and electrochemical deposition. The Cu layer thickness was varied to study the resulting differences in coercivity and magnetization reversal. Magnetization versus field loops both parallel and perpendicular to an applied field were measured to investigate the mechanisms of magnetization reversal. It was found that the coercivity decreased with increasing Cu thickness. In addition, the magnetization reversal appeared to be a combination of rotation and spin flipping, which was dependent on the Cu thickness and on the angle of the nanowires with the applied field.

The microstructure in a small amount of Al2O3-doped Y2O3-stabilized tetragonal zirconia polycrystal (Y-TZP) sintered at 1100–1650 °C was examined to clarify the effect of Al3+ ions segregated at grain boundaries on cubic-formation and grain-growth processes. The sintering rate in Y-TZP was remarkably enhanced by Al2O3-doping. In addition, at temperatures >1500 °C, grain growth remarkably proceeded, and the fraction of the cubic phase increased in comparison with that of undoped Y-TZP. High-resolution electron microscopy and nanoprobe x-ray energy dispersive spectroscopy measurements revealed that no amorphous layer existed along the grain-boundary faces in Al2O3-doped Y-TZP and that Y3+ and Al3+ ions segregated at grain boundaries over widths of ∼10 and ∼6 nm, respectively. At 1100 °C, Al3+ ions started to segregate at grain boundaries, and the segregation peak of Al3+ ions increased as the sintering temperature increased. Cubic-formation and grain-growth behaviors in Al2O3-doped Y-TZP were reasonably interpreted by taking into account the effect of Al3+ ions segregating along grain boundaries.

Homogeneous ∈-iron nitride powder particles of the compositions Fe3N1.00, Fe3N1.22, Fe3N1.30, and Fe3N1.39 were investigated using selected-area electron diffraction. The superstructure reflections, due to N ordering on the octahedral interstitial sites of a hexagonal close-packed (hcp) arrangement of Fe, indicate a hexagonal supercell with a′ = 31/2ahcp, c′ = chcp for all cases; P6322 space group symmetry for Fe3N1.00, Fe3N1.30, and Fe3N1.39; and lower symmetry (P312) for Fe3N1.22 and some of the Fe3N1.30 particles. Recognition of the occurrence of double diffraction is essential for correct interpretation of the diffraction patterns. Additionally, diffuse scattering by some of the Fe3N1.39 grains was observed.

Lead titanate (PbTiO3) nano- and microtubes were fabricated by wetting ordered porous alumina and macroporous silicon with precursor oligomers coupled with templated thermolysis. The diameters of the PbTiO3 tubes range from a few tens of nanometers up to one micron. The proper selection of the template allowed for a precise adjustment of their size over two orders of magnitude. Electron microscopy and x-ray diffraction revealed that the tube walls were polycrystalline. The generic approach presented here can be adapted for the fabrication of tubes and rods from a multitude of functional inorganic oxides.

Mesoporous barium titanate powders having a 100- to 300-nm size were prepared by hydration and condensation of titanium tetra-isopropoxide and barium precursors in the presence of an organic surfactant, tetradecylamine, which was used as a self-assembly micelle. The processing and sintering of these mesoporous barium titanate powders has been investigated. X-ray diffraction, scanning electron microscopy, and transmission electron microscopy were used to identify the structural characteristics and morphologies of the powders. Mesoporous wormhole-like powders with surface areas around 53 ∼ 108 m2/g could be obtained after removing the micelle organics by calcination at 400 °C for 3 h. Powders derived using barium hydroxide were found to form a larger pore size and a higher surface area. The addition of acetic acid was also effective in increasing the surface area. A formation mechanism for the mesoporous structure is depicted. Heat treatment caused the mesoporous spheres to shrink, and 155- ∼ 330-nm grain sizes were readily obtained after pressureless sintering at 900 ∼ 1000 °C for 1 h in air.

Microstructure-related local deformation behavior was evaluated using nanoindentation techniques for a type 316 austenitic stainless steel used in energy generation plants. The sample was aged for 39,332 h (4.5 years) at 700 °C. The microstructure included the σ phase precipitated at grain boundaries and in grain interiors. The nanohardnesses of the σ phase and the matrix in the aged and virgin samples were evaluated quantitatively. The hardness of the σ phase was found to be extremely high in the order of 17 GPa, which is much higher than the value of about 3.4 GPa for the matrix in the aged sample. The hardnesses of the σ phase at the grain boundary and the adjoining matrix were the same as those in the grain interior. Moreover, the hardness of the matrix of the aged sample was about 30% lower than that of the virgin sample while the Vickers hardness as a macroscopic strength of the aged sample was about 45% higher than that of the virgin one. The deformation and fracture behavior in a local region was discussed in terms of the inhomogeneous mechanical properties in the multi-phase microstructure.

Ionic polymer metal composite (IPMC) is a promising candidate for artificial muscles and other bio-related applications. Compared with the widely reported Nafion, Flemion-based IPMC has some more attractive advantages. To improve its mechanical stability in dry environments, the organic solvent glycerol was applied. The mechanical characteristics such as tip displacement, tip force and durability were measured and analyzed. The results showed that Flemion-based IPMC with glycerol as solvent has optimum mechanical stability in dry conditions and will be a good candidate for artificial muscles working in air.

We present a detailed study of the thermal stability of organic thin films of diindenoperylene encapsulated by sputtered aluminum oxide layers. We studied the influence of capping layer thickness, stoichiometry, and heating rate on the thermal stability of capped films and their eventual breakdown. Under optimized encapsulation conditions (thick and stoichiometric capping layer), the organic films desorb only at temperatures 200 °C above the desorption of the uncapped film. Moreover, the capped organic films retain their crystalline order at these elevated temperatures, whereas they would normally (i.e., uncapped) be in the gas phase. This study therefore also shows a way of studying organic materials under temperature conditions normally inaccessible. Considering results from complementary techniques, we discuss possible scenarios for the eventual breakdown. The results have implications for the performance and long-term stability of organic devices for which stability against elevated temperatures as well as against exposure to ambient gases is crucial.

A silica-free MgO–CaO–BaO–Al2O3–ZrO2 glass was converted into glass-ceramic by adding zirconia as a nucleating agent. The crystallization and properties of the glass-ceramics were investigated. It was found that ZrO2 is an efficient nucleating agent for the present calcium aluminate glass. Addition of an appropriate amount of ZrO2 changed the crystallization behavior from surface nucleation to internal nucleation. The primary crystalline phase was Ca3Al2O6, which exhibited bulk nucleation. When the crystallizing time was increased, BaAl2O4 formed as a surface layer that grew from the surface into the interior of the sample. The hardness was increased when the parent glass was converted into glass-ceramics. The glass-ceramics without BaAl2O4 surface layer have visible-to-infrared transparency comparable with the parent glass. The transparency was substantially reduced after the development of the surface layer.

Immobilization of titania nanoparticles on submicron-sized silica carrier spheres was achieved, and the relevant photocatalytic efficiency was studied. In contrast to the commonly adopted practice of either free suspending nano-sized catalyst particles or immobilized catalyst particles on large supports for photocatalytic applications, the present approach offers a third option, avoiding the disadvantages of the above-mentioned two practices. In the model system of photo-degradation of methylene blue, the photocatalytic efficiency of the present catalyst form was found comparable to that of free-suspending P25 nanoparticles, a popular commercial titania photocatalyst, of the same total catalyst surface area. The present photocatalytic process was found to be diffusion dominant, and its impressive catalytic performance was attributed to the well-separated, smaller than usual titania particles immobilized on the surfaces of submicron-sized silica spheres.

Three-dimensional simulations for relieving the current crowding effect in solder joints under current stressing were carried out using the finite element method. Three possible approaches were examined in this study, including varying the size of the passivation opening, increasing the thickness of Cu underbump metallization (UBM), and adopting or inserting a thin highly resistive UBM layer. It was found that the current crowding effect in the solder bump could be successfully relieved with the thick Cu UBM or with the highly resistive UBM. Compared to the solder joint with Al/Ni(V)/Cu UBM, for instance, the maximum current density in a solder bump decreased dramatically by a factor of fifteen, say from 1.11 × 105 A/cm2 to 7.54 × 103 A/cm2 when a 20-μm-thick Cu UBM was used. It could be lowered by a factor of seven, say to 1.55 × 104 A/cm2, when a 0.7-μm UBM of 14770 μΩ cm was adopted. It is worth noting that although a resistive UBM layer was used, the penalty on overall resistance increase was negligible because the total resistance was dominated by the Al trace instead of the solder bump. Thermal simulation showed that the average temperature increase due to Joule heating effect was only 2.8 °C when the solder joints with UBM of 14770 μΩ cm were applied by 0.2 A.

The effect of growth conditions on the composition and structure of Si1−xGex nanowires grown by the vapor–liquid–solid method using gaseous precursors (SiH4 and GeH4) was investigated. Transmission electron microscopy was used to characterize the structural properties and elemental composition of the nanowires. At higher growth temperatures (>425 °C), Ge thin film deposition on the nanowire surface resulted in Au loss during growth and the formation of tapered structures. By simultaneously reducing the growth temperature from 425 to 325 °C to suppress the rate of Ge film deposition and increasing the GeH4/(GeH4 + SiH4) gas ratio, Si1−xGex nanowires were produced with Ge fractions spanning the entire composition range. The Ge fraction follows that predicted from the elemental nanowire growth rates in the Ge-rich (x > 0.5) regime, but deviates to higher Ge fractions in Si-rich (x < 0.5) nanowires. A mechanism was proposed whereby surface diffusion provides an additional pathway to Ge incorporation in Si-rich Si1−xGex nanowires.