Electron-beam-induced effects in preamorphized Sr2Nd8(SiO4)6O2 were investigated in situ using transmission electron microscopy with 200-keV electrons at temperatures ranging from 380 to 780 K. Within the electron-irradiated area, epitaxial recrystallization was observed from the amorphous/crystalline interface toward the surface, with the rate of recrystallization increasing as temperature increased from 380 to 580 K. Structural contrast features (i.e., O deficient amorphous material), as well as recrystallization, were observed outside of the irradiation area at temperatures from 680 to 780 K. Ionization-induced processes and local nonstoichiometry induced by oxygen migration and desorption are possible mechanisms for the electron-beam- induced recrystallization and for the formation of the structural contrast features, respectively.

New porous biomaterials based on hydroxyapatite (HAp) were designed as obturation materials for dental cavities. Synthetic HAp powder with a particle diameter of 150 μm was agglutinated using three different polyurethane monocomponents (rigid, semi-rigid, and flexible), enabling the matching of their properties to those of real teeth. Alumina particles were also added in some cases. Our new hybrid materials contain up to 60% HAp. Interconnected pores range in size from 100 to 350 μm, while the pore volume fraction varies between 25% and 60%. Most of these materials possess the right morphology for implants and prostheses because their porous structures can be vascularized for bone and tooth ingrowth. Some samples also contain alumina particles to improve the abrasion resistance and to support the stresses produced during mastication. The materials were characterized by x-ray diffraction, scanning electron microscopy, and mechanical testing, along with abrasion, scratch, sliding wear, friction, and staining tests.

Transmission electron microscopy (TEM) and fast Fourier transformation (FFT) analysis were used to examine the microstructures of amorphous carbon (a-C) films deposited on Si(100) by radio-frequency (rf) sputtering without magnetron. TEM analysis revealed that a-C films synthesized under certain deposition conditions contained randomly dispersed nanocrystallites ∼35 Å in size. FFT results indicated that the nanocrystallites possessed diamondlike cubic structures with their close-packed {111} planes parallel to the film surface. The formation of diamondlike nanocrystallites is attributed to metastable carbon atom clusters of trigonal carbon hybridization that were sputtered off from the graphite target under certain process conditions. Cluster distortion upon deposition onto the growing film surface by the bombarding Ar+ ions promoted tetrahedral carbon atom hybridization and, possibly, epitaxial growth of diamondlike nanocrystallites for a short duration.

Diatoms are well known for the intricately patterned nanostructure of their silica-based cell walls. To date, the optical properties of diatom cell-wall ultrastructures have largely gone uncharacterized experimentally. Here we report the results of a detailed experimental investigation of the way in which light interacts with the ultrastructure of a representative centric diatom species, Coscinodiscus wailesii. Light interaction both with individual valves and whole bivalves of the diatom C. wailesii was measured. Significant sixfold symmetric diffraction through the valve ultrastructure was observed in transmission and quantified to efficiencies that were found to be strongly wavelength dependent; approximately 80% for red, 30% for green, and 20% for blue light. While these results may potentially offer insight into the role of periodic nanostructure in diatom selection, they are also important for consideration in the design of biomimetic optics-based diatom applications.

Biomimetic layer-by-layer (BioLBL) is a layering method in which the binding and mineralization activities of a peptide aptamer are alternately used to accumulate layers of aptamer-displaying nanomaterials and thin mineral strata. We previously demonstrated this in aqua nanofabrication with BioLBL using a recombinant ferritin that displays an aptamer for titanium (minTBP-1) [K. Sano et al.: J. Am. Chem. Soc. 128, 1717 (2006); K. Sano et al.: Nano Lett.7, 3200 (2007)]. To expand the versatility of BioLBL, here we prepared a modified ferritin that was chemically ornamented with minTBP-1 and showed that BioLBL enables the formation of multiple layers of the chemically modified ferritin in a stepwise manner.

Gold particles were fabricated by the high-intensity femtosecond laser irradiation of gold (III) chloride trihydrate (HAuCl4) aqueous solution. The structure and size distribution of the prepared particles were evaluated by transmission electron microscopy. The configuration of the gold particles varied with the concentration of the HAuCl4 aqueous solution. The mean particle size and size distribution were changed by the addition of polyvinylpyrrolidone (PVP), which acted as a dispersant, and monodispersed gold nanoparticles with a diameter of about 3 nm were successfully fabricated. The formation process of the nanoparticles is discussed in terms of the optical decomposition of molecules in the highly intense optical field generated by femtosecond laser irradiation.

Palladium hydrides have important applications. However, the complex Pd–H alloy system presents a formidable challenge to developing accurate computational models. In particular, the separation of a Pd–H system to dilute (α) and concentrated (β) phases is a central phenomenon, but the capability of interatomic potentials to display this phase miscibility gap has been lacking. We have extended an existing palladium embedded-atom method potential to construct a new Pd–H embedded-atom method potential by normalizing the elemental embedding energy and electron density functions. The developed Pd–H potential reasonably well predicts the lattice constants, cohesive energies, and elastic constants for palladium, hydrogen, and PdHx phases with a variety of compositions. It ensures the correct hydrogen interstitial sites within the hydrides and predicts the phase miscibility gap. Preliminary molecular dynamics simulations using this potential show the correct phase stability, hydrogen diffusion mechanism, and mechanical response of the Pd–H system.

Crystalline samples of zinc oxide on a mesoporous amorphous silica substrate were prepared by 5 to 15 atomic layer deposition cycles with diethyl zinc and water at 150 °C. Samples were characterized by x-ray diffraction, thermogravimetry, and nitrogen adsorption–desorption isotherms. High-temperature oxide melt solution calorimetry and water adsorption calorimetry experiments were performed to measure surface enthalpy for crystalline ZnO particles supported on the substrate. The measured enthalpies 1.23 ± 0.35 and 2.07 ± 0.59 J/m2 for hydrous and anhydrous surfaces, respectively, are in agreement with previously reported measurements for unsupported ZnO nanoparticles. Feasibility of thermochemical characterization of complex system of atomic layer deposition (ALD) prepared particles on a substrate was demonstrated.

Texture evolution of a commercial-purity titanium (CP-Ti) during cold rolling was studied by means of x-ray diffraction (XRD) and electron back-scattered diffraction (EBSD). Twinning was identified to significantly contribute to deformation up to reductions of about 50%. Based on initial texture of the material investigated and twinning modes available in hexagonal close-packed (HCP) structures, the measured texture evolution can be interpreted in terms of (i) compressive twinning ({11¯22}〈11¯2¯3〉) within the two dominant initial texture components B ({0001}〈10¯10〉±40°TD) and E ({0001}〈11¯20〉±40°TD) and (ii) followed by tensile twinning ({10¯12}〈10¯1¯1〉) in the then-favorably reoriented twinned part. Reduction of grain size at high deformation inhibits further twinning and results in a stable texture evolution driven exclusively by dislocation slip. During cold rolling, the crystals of the initial texture component B first rotate to orientation M ({01¯10}〈2¯1¯12〉) by compressive twinning (primary), and then orientation M rotates to orientation D ({0001}〈11¯20〉) by tensile twinning (secondary). Meanwhile, the crystals of the initial component E first rotate to the orientation M′ ({14¯53}〈6¯5¯13〉) by compressive twinning (primary), and then orientation M′ rotates to the orientation A ({0001}〈10¯10〉) by tensile twinning (secondary). At higher deformation level, twinning was significantly depressed by strongly refined grain size, which resulted in the elimination of the transient texture components caused by slip. These results are useful for the prediction and control of the texture in titanium.

The mechanical properties of Zr52.5Ni14.6Al10Cu17.9Ti5 and Ti40Zr25Ni3Cu12Be20 metallic glasses were investigated under uniaxial compressive loading and small punch loading, respectively. The Zr-based metallic glass displays higher density of shear bands, larger critical shear offsets and higher energy absorbing capability than the Ti-based metallic glass under the small punch tests. A concept of critical shear offset is proposed to explain the difference in shear deformation abilities or plasticity of different metallic glasses. The current experiments demonstrate that, in contrast with the small difference between the responses of the Zr- and Ti-based metallic glasses under uniaxial compressive loading, the biaxial tension produced by the small punch test is an effective way to evaluate the difference in shear deformation abilities and can be used to distinguish the brittleness or plasticity of various metallic glasses.

In a compression test for a Zr-based bulk metallic glass, a dominant shear band was preserved before fracture by a cylindrical stopper. A heat-affected zone (HAZ) ∼10 μm thick together with shear band was discovered in the center of the deformed sample by preferential ion milling. By using a low aspect ratio sample for compression, diverse micron-scaled HAZs among multiple shear bands were also revealed. Based on above experimental results and the isothermal source model, it was found that the thickness of shear band and its HAZ increased continuously with the progression of shear deformation.

The molecular dynamics method has been used to simulate mode I cracking in Ni3Al. Close attention has been paid to the process of atomic configuration evolution of the cracks. The simulation results show that at low temperature, the Shockley partial dislocations are emitted before the initiation of the crack propagation, subsequently forming the pseudo-twins on (111) planes in crack-tip zone, and then the crack cleavage occurs. The emitting of the Shockley partial dislocations accompanies the crack cleavage during the simulation process. At the higher temperature, the blunting at the crack tip is caused by the [110] superdislocations emitted on (100) plane. The present work also shows that the dipole dislocations on (111) planes in the 1/2[110] dislocation core can be formed.

Following the discussion of modeling grain refinement in Part I, [X. Yao, et al., J. Mater. Res.23(5), 1282, the effect of Al–Ti–B master alloy additions on grain formation in commercial-purity (CP) aluminum was investigated. The characteristics of the addition particles as applicable to the model are presented. The effect of adding TiB2 particles, the introduction of extra particles by reactions in the melt, and the effect of adding extra solute Ti are all modeled. The distribution of the potential particles and its effect on grain formation was also modeled to establish the relationship between the grain size and microstructure morphology and the additive characteristics. The calculated results are comparable with experimental data. Accordingly, possible mechanisms of grain refinement with Al–Ti–B refiners were proposed.

In situ scanning electron microscope observations have been performed on passivated damascene Cu interconnect segments of different widths during accelerated electromigration tests. In some cases, voids form and grow at the cathode. However, an alternative failure mode is also observed, during which voids form distant from the cathode end of the interconnect segment and drift toward the cathode, where they eventually lead to failure. The number of observations of this failure mode increased with increasing linewidth. During void motion, the shape and the velocity of the drifting voids varied significantly. Postmortem electron backscattered diffraction (EBSD) analysis was performed after in situ testing, and a correlation of EBSD data with the in situ observations reveals that locations at which voids form, their shape evolution, and their motion all strongly depend on the locations of grain boundaries and the crystallographic orientations of neighboring grains.

A pushout test method was used to quantify effect of thermal cycling temperatures on the delamination toughness of an electron beam physical vapor deposited thermal barrier coating (EB-PVD TBC). The delamination toughness, Γi, was related to the maximum thermal cycling temperature, Th, equal to 1000, 1025, 1050, and 1100 °C. The measured delamination toughness varied from 9 to 95 J/m2. At Th = 1000 °C, Γi attained a maximum value, larger than that of the as-deposited sample and decreasing with increased Th. During the thermal cycling tests, the thermally grown oxide (TGO) was formed between the TBC and the bond coat deposited onto the superalloy substrate. Inside the TGO layer, mixture of Al2O3 and ZrO2 oxides was observed close to the TBC side with nearly pure Al2O3 phases close to the bond-coat side. During the pushout test, delamination occurred at the interface of the mixture and pure Al2O3 layer with an exception for Th = 1100 °C specimens where delamination also occurred at the interface between the TGO and bond-coat layers. The effect of thermal cycling temperatures on the delamination toughness is discussed in terms of the microstructural change and delamination behavior.

The effects of salient testing parameters on four-point adhesion measurements of thin-film structures on silicon substrates were systematically studied. These included specimen geometry, applied displacement rate, and load point separation. Measured fracture energy values, Gc, were observed to increase as the ratio of applied moment arm to specimen thickness was decreased beyond a value of ∼4, particularly for specimens with Gc > 5 J/m2. Testing parameters that affect the steady-state crack velocity were also found to affect reported Gc values. The resulting trends in Gc values are shown to be related to loading-point friction and environmentally assisted cracking effects. Good practice testing guidelines are suggested to improve the accuracy and precision of four-point bend measurements.

The synthesis of ultrafine tungsten carbide (WC) powder has been investigated from a WO3 + Mg + C mixture via combustion technique. The values of combustion parameters were estimated over the Mg concentration range 3 to 16 mol. Fast increasing tendency of the WC/W2C phase ratio from Mg concentration has been found in the final products. Phase pure WC was prepared with more than 10 mol Mg, and a small amount of ammonium carbonate (or urea) was blended with the WO3+ C mixture. The effects of the combustion conditions on product morphology and composition were evaluated using scanning electron microscopy and x-ray diffraction analysis. The results of the investigation indicate that carbon-containing compounds significantly enhance the combustion synthesis process; leading to higher conversion efficiencies and phase pure WC formation at 1500–1550 °C. The crystalline particles of WC showed a narrow distribution in particle size, with a mean diameter around 200 nm. The results are discussed in the context of gas-phase and solid-phase transport models.

Anomalous eutectics in the solidification structure of undercooled Ni–18.7 at.% Sn eutectic alloy were examined by optical metallography and electron backscattered diffraction. It was revealed that α–Ni particulates are, in principle, randomly distributed in the anomalous eutectics in the undercooling range investigated. Another eutectic phase, β–Ni3Sn, is well orientated at low undercoolings but gradually becomes inconsistent in orientation as undercooling increases, accompanied by an increasing number of grain boundaries in it. As the solidification structure changes from a mixture of anomalous eutectics plus lamellar eutectics to full anomalous eutectics beyond a critical undercooling of 130 K, however, misorientation in the β–Ni3Sn phase disappears completely from the measurement area. Partial remelting of the primary solid was proposed to be the origin of the anomalous eutectic formation, and quantitative analyses were performed.

In this work, we report a method to synthesize a peculiar composite structure of tubular carbon nanofibers (CNFs) growing on a microsized tin (Sn) whisker. The material used is a commercially available copper clad laminate (CCL). The CCL is composed of a surface copper (Cu) layer and a bottom polymer (phenol-formaldehyde resin) board, in which the polymer board is used as the carbon source. Using lithography and lift-off techniques, the Cu layer was patterned to a stripelike Cu trace. A Sn thin film was then evaporated on the polymer board near the Cu trace. To release the residue stress that resulted from the evaporation; Sn whiskers with diameters of about 2 to 5 μm were formed on the Sn thin film after evaporation. By passing an electric current through the Cu trace, the Cu trace was heated due to Joule heating and served as a heating source for the thermal decomposition of phenol-formaldehyde. After heat treatment, the CNFs grew on the surface of the Sn whiskers with tubular hollow-cored structure. The diameter of the tubular CNFs is about hundreds of nanometers and their length can reach several micrometers. The growth mechanism of the brushlike composite structure is also discussed.

Dynamic indentation techniques are often used to determine mechanical properties as a function of depth by continuously measuring the stiffness of a material. The dynamics are used by superimposing an oscillation on top of the monotonic loading. Of interest was how the oscillation affects the measured mechanical properties when compared to a quasi-static indent run at the same loading conditions as a dynamic. Single crystals of nickel and NaCl as well as a polycrystalline nickel sample and amorphous fused quartz and polycarbonate have all been studied. With respect to dynamic oscillations, the result is a decrease of the load at the same displacement and thus lower measured hardness values of the ductile crystalline materials. It has also been found that the first 100 nm of displacement are the most affected by the oscillating tip, an important length scale for testing thin films, nanopillars, and nanoparticles.