The high-temperature indentation fracture and microstructures of dysprosium niobate (DyNbO4) were investigated by optical, scanning, and transmission electron microscopy (OM, SEM, and TEM). Polycrystalline samples were sintered at 1350 °C for 3 h and cut into 3 mm disks for TEM. The disks were indented in a Nikon QM (Tokyo, Japan) hot hardness indenter at room temperature up to 1000 °C. Many lamellar twins having different widths were observed by TEM as well as intergranular microcracks. The room temperature hardness was relatively low at 5.64 GPa and decreased with elevated temperatures. Crack lengths were short, showing a typical micro-cracking effect. In the sample indented at 1000 °C, dislocations in periodic arrays were evident, and their density increased markedly due to heavy plastic deformation.

A new patterning technique for the deposition of sol-gels and chemical solution precursors was developed to address some of the limitations of soft lithography approaches. When using micromolding in capillaries to pattern precursors that exhibit large amounts of shrinkage during drying, topographical distortions develop. In place of patterning the elastomeric mold, the network of capillary channels was patterned directly into the substrate surface and an elastomer membrane is used to complete the channels. When the wetting properties of the substrate surfaces were carefully controlled using self-assembled monolayers (SAMs), lead zirconate titanate thin films with nearly rectangular cross-sections were successfully patterned. This technique, called microchannel molding (μCM), also provided a method for aligning multiple layers such as bottom electrodes for device fabrication.

Detailed sintering studies have been carried out on attrition milled nanocrystalline titanium powder through isothermal dilatometry over a temperature range of 300–1250 °C along with microstructural and x-ray diffraction studies. The sintering behavior of attrition milled nanocrystalline titanium appears to be characterized by: (i) very low activation energies, (ii) high shrinkage anisotropy, (iii) very rapid grain growth in the beta range, and (iv) two kinds of densification processes, namely, intra-agglomerate and inter-agglomerate. Analysis of the kinetic data through sintering diagram approach indicates the operation of particle sliding and grain boundary rotation, type of mechanism in addition to the grain-boundary diffusion, and lattice diffusion as the dominant mass transport mechanisms.

The commercial nickel base alloy NIMONIC PE16 is strengthened by nano-scale spherical coherent precipitates of the intermetallic γ′-phase Ni3(Al,Ti). A bulk polycrystalline specimen of NIMONIC PE16 was aged such that it was in the transition range from the peak- to the overaged state. This transition limits the duration of technically useful aging treatments of structural particle strengthened materials. Thin foils prepared from this specimen were stretched inside a transmission electron microscope, and the dislocation processes were observed under full load. Two dislocations with identical Burgers vectors of the type 1/2〈110〉 form a pair and glide together. The leading 1/2〈110〉 dislocation bypasses the γ′-precipitates and the trailing one shears them. These dislocation processes are also discussed with reference to the results of computer simulations.

Raman spectroscopy was used to determine the lattice expansion and stress distribution within the ion implanted layer in sapphire crystals. The crystals with the (1120) facewere implanted with 3.0 MeV H+ ions to doses of 3.3 × 1017 cm−2 and 4.8 × 1017 cm−2.The strain components and their variation with depth were analyzed by measuring the shift of the Raman peak on the cross-sectional basal plane. A continuum mechanics approach considered a model of a semi-infinite anisotropic elastic space subjected to the implantation-induced lattice expansion. The expansion and resulting compressive stresses were found to increase with depth, reaching a sharp maximum at the end of the ion range. The implantation-induced expansion coefficient was shown to be independent of the ion energy loss and implantation depth in sapphire. Such behavior was discussed in light of stopping and range of ions in matter data and defect production by nuclear collisions and ionization processes.

Hollow and nanoporous particles of zero-valent iron (ZVI) were prepared with template-directed synthesis. Polymer resin beads (0.4 mm diameter) were coated with nanoscale iron particles by reductive precipitation of ferrous iron [Fe(II)] with sodium borohydride. The resin was calcinated at 400 °C to produce hollow and nanoporous iron spheres. The nanoporous iron oxides were then reduced to metallic iron by hydrogen at 500 °C. Scanning electron microscope images of the reduced iron spheres showed that the particles were hollow. The shell thickness was approximately 5 μm and highly porous. Brunauer–Emmett–Teller specific surface area was 2100 m2/kg. In comparison, the theoretical specific surface area of solid iron particles of the same size is just 1.9 m2/kg. Batch tests showed that the surface area normalized reactivity of the porous particles were 14–31% higher than microscale iron particles with similar surface areas for the transformation of hexavalent chromium [Cr(VI)], azo dye Orange II {4-[(2-hydroxyl-1-naphthalenyl)azo]-benzenesulfonic acid monosodium}, and trichloroethene. The combined performance enhancement (larger surface area and higher surface activity) is significant (>1200 times).

We report the formation of microstructure- and property-controllable Nd60Al10Ni10Cu20−xFex (0 ≤ x ≤ 20) alloys by varying the content of Fe element. The microstructure of the Nd-based alloy can be changed progressively from a full glassy state into a composite state with nanocrystalline particles in the glassy matrix and, finally, into a nanostructured state, accompanied by variation in magnetic property gradually from paramagnetic to hard magnetic. The role of Fe addition in the control of microstructure and magnetic property is clarified. We expect that the results would have implication in the development of the microstructure- and property-controllable functional materials for various applications.

Time-resolved photo- and thermoelectric effects (TTE) were used to determine simultaneously trap levels and trap state density differences in amorphous (a-SiGe:H) samples. In particular, the trap state density differences are obtained from the decay of the ambipolar charge distribution (i.e., stage II of the TTE transients). This type of spectroscopy has been applied for the first time to a-SiGe:H samples, and indeed trap states that seem to relate to concentration fluctuations, that is, Si(Ge) and Ge(Si) clusters, are observed.

Explosive shock compaction was used to consolidate powders obtained from melt-spun Pr2Fe14B/α–Fe nanocomposite ribbons, to produce fully dense cylindrical compacts of 17–41-mm diameter and 120-mm length. Characterization of the compacts revealed refinement of the nanocomposite structure, with approximately 15 nm uniformly sized grains. The compact produced at a shock pressure of approximately 1 GPa maintained a high coercivity, and its remanent magnetization and maximum energy product were measured to be 0.98 T and 142 kJ/m3, respectively. The compact produced at 4–7 GPa showed a decrease in magnetic properties while that made at 12 GPa showed a magnetic softening behavior. However, in both of these cases, a smooth hysteresis loop implying exchange coupling and a coercivity of 533 kA/m were fully recovered after heat treatment. The results illustrate that the explosive compaction followed by post-shock heat treatment can be used to fabricate exchange-coupled nanocomposite bulk magnets with optimized magnetic properties.

When determining elastic modulus and hardness of viscoelastic-plastic materials by depth-sensing indentation, one must respect their specific response. In the monotonic load-unload testing mode, the unloading should be preceded by a dwell mitigating the influence of the delayed deforming. The continuous stiffness measurement (CSM) mode, with a small harmonic signal added to the basic monotonic load, enables continuous measurement of harmonic contact stiffness and mechanical properties as a function of depth. However, the contact depth and area in this mode actually depend on the slow (monotonic) component of the loading and should be determined not from the harmonic contact stiffness but from the unloading stiffness; otherwise, the calculated elastic modulus and mean contact pressure will be incorrect. This paper provides the formulae for these calculations, defines special characteristics—such as apparent dynamic hardness and the index of sensitivity to harmonic loading—and shows how to improve results by smoothing the harmonic stiffness curve. The proposed methods are illustrated through nanoindentation tests of polymethyl methacrylate.

A systematic investigation and comparison of the photoluminescence (PL) quantum yields of six erbium(III) organic complexes are reported. We demonstrated that the PL quantum yield could be significantly improved by getting rid of OH and CH groups in the complexes. Moreover, perfluooctanoic acid with neither OH nor CH groups was used as a ligand to form complex with Er3+. The quantum yield of the newly synthesized erbium(III) complex was found to be as high as 2%, 100 times higher than ever reported.

The hollow mesoporous spheres (HMS) with cubic pore network have been synthesized via a simple two-step method. Two drugs of different molecules size, Aspirin and Gentamicin, were tested by one simple adsorption process. Up to 336 mg Aspirin molecules can be stored in 1.0 g HMS, while Gentamicin molecules of much larger size are much more difficult to be introduced into the pore channels of HMS. The same results can be obtained by using MCM-48 and MCM-41 as comparative mesoporous carriers. The HMS shows significantly higher storage amount of Aspirin than conventional MCM-48 and MCM-41 due to its hollow core structure. The release process of HMS-Aspirin, MCM-48-Aspirin and MCM-41-Aspirin are found to have a sustained-release property and follow a Fickian diffusion mechanism. Moreover, the HMS is suitable for storage of drug molecules of much smaller size.

Work on nitrogen loss and structural change of nitrogen-containing SBA-15 mesoporous materials after heat treatment in air or water treatment is described herein. The nitrogen-containing SBA-15 lost nitrogen after being treated in air at high temperature or in water, the mesoporous structure of which was very well maintained and did not collapse. HRTEM, N2 sorption, powder XRD, and SEM were used to study the structural ordering and morphology of the mesoporous silicon oxynitride materials before and after treatment. FTIR and C/N/H elemental analysis confirmed that nitrogen loss occurred after the mesoporous silicon oxynitride material was treated. Nitrogen was lost via hydrolysis of ammonium groups when mesoporous silicon oxynitride material was treated in water and by being substituted by oxygen from air when it was heated in air at high temperature.

Lead zirconate titanate (PZT) films of composition close to the morphotropic phase boundary were deposited onto standard Si/SiO2/Ti/Pt substrates using a modified sol-gel process. The preparation conditions were optimized to obtain high-quality films at sufficiently low temperature (Ta - 500 °C). The dielectric, ferroelectric, and piezoelectric properties of the films were then measured as a function of the annealing temperature and the number of distillations to evaluate their suitability for micromechanical applications. The maximum values of the longitudinal charge and voltage piezoelectric coefficients were d33 ∼ 65 pm/V and g33 ∼ 4 × 10−3 Vm/N, respectively. The results indicate that the piezoelectric properties improved and became saturated with increasing number of distillations and are almost independent on Ta. Only moderate decrease of the piezoelectric response with frequency suggests that the investigated PZT films can be used in high-frequency piezoelectric applications. The results are discussed in terms of the microstructure and interface effects on the piezoelectric deformation in ferroelectric thin films.

In this paper, we present a method for determining the initial contact point and nanoindentation load–indentation depth characteristics for soft materials. The method is applied to the prediction of the load–indentation depth characteristics of polydimethylsiloxane. It involves the combined use of Johnson–Kendall–Roberts and Maugis–Dugdale adhesion theories and nonlinear least squares fitting in the determination of the initial contact point, the transition parameter, and the contact radius at zero contact load. The elastic modulus and the work of adhesion are also extracted from the load–indentation depth curves.

In this study, the transport of water-stable “nano-C60 particles” (a term used to refer to underivatized C60 crystalline nanoparticles, stable in water for months) through a soil column (packed with Lula soil, 0.27% organic carbon) was investigated for the first time. Nano-C60 particle breakthrough experiments were conducted at different flow rates, while other column operating parameters remained fixed through all the experiments. Nano-C60 particles were observed to be more mobile at higher flow velocity: at the flow velocity of 0.38 m/d, the maximum percent of nano-C60 breakthrough (C/C0) was 47%; at the flow velocity of 3.8 m/d, the plateau value of nano-C60 breakthrough was 60%; and at the flow velocity of 11.4 m/d, the plateau value of nano-C60 breakthrough was almost 80%. At the low flow velocity (0.38 m/d), which is typical of groundwater flow, nano-C60 particles showed very limited mobility: after about 57 pore volumes, they deposited to the soil column so rapidly that virtually no nano-C60 was detected in the effluent. This observed “favorable deposition” (attachment efficiency α = 1) was probably due to “filter ripening.” Also the release of nano-C60 particles after flow interruption was observed. The transport of naphthalene through the same soil column containing 0.18% nano-C60 particles deposited was measured. A retardation factor of about 13 was observed, possibly suggesting that sorbed nano-C60 particles in the soil column sorbed naphthalene similar to soil organic carbon. An asymmetric naphthalene breakthrough curve was observed, which is possibly due to “sorption nonequilibrium.”

Polyvinylpyrrolidone (PVP) reduction effect on free and complex Ag+ and Au3+ ions was studied from optical measurements by adding a metal precursor (K-30), commonly used as a stabilizer, to PVP. It was found that PVP has a strong reduction effect on free ionic metal, such as Ag+ ion in AgNO3, but much weaker on complex ionic metals, AuCl4− in HAuCl4 and Ag(NH3)2+ in Ag(NH3)2OH. This is explained based on the coordinative field of polar group in PVP molecules.

To understand the ceria–silica chemical mechanical polishing (CMP) mechanisms, we studied the effect of ceria slurry pH on silica removal and surface morphology. Also, in situ friction force measurements were conducted. After polishing; atomic force microscopy, x-ray photoelectron spectroscopy, and scanning electron microscopy were used to quantify the extent of the particle–substrate interaction during CMP. Our results indicate the silica removal by ceria slurries is strongly pH dependent, with the maximum occurring near the isoelectric point of the ceria slurry.

As layer thickness of multilayer ceramic capacitors decreases, nanoparticles of high dielectric materials, especially BaTiO3, are needed. Tabular metal nanoparticles produce thin metal layers with low surface roughness via electrophoretic deposition. To achieve similar results in dielectric layers requires the synthesis and dispersion of tabular BaTiO3 nanoparticles. In the current study, the synthesis of BaTiO3 was investigated using a hydrothermal route. Transmission electron microscopy and atomic force microscpy analyses show that the synthesized particles are single crystal with a 〈111〉 zone axis and a median thickness of 5.8 nm and face diameter of 27.1 nm. Particle growth is likely controlled by the formation of {111} twins and the synthesis pH, which stabilizes the {111} face during growth. With limited growth in the 〈111〉 direction, the particles develop a platelike morphology. Physical property characterization shows the powder is of high purity with low hydrothermal defect concentrations and controlled stoichiometry.

The crystallization and phase transformations of amorphous NiTi thin films were studied using in situ transmission electron microscopy (TEM). These films were sputter-deposited onto micromachined silicon-nitride membranes and subjected to heating and cooling conditions. The microstructural evolution was monitored and recorded. Kinetic parameters such as the nucleation rate, growth rate, and area-fraction transformed were independently determined by noting the number of grains per frame and their change in size. Using the Johnson–Mehl–Avrami–Kolmogorov analysis, fitted kinetic parameters were determined and found to be consistent with TEM observations. To explore the compositional sensitivity of crystallization, samples near-equiatomic and slightly Ti-rich were studied with these methods. TEM micrographs show that equiatomic films exhibit polymorphic crystallization while samples that are slightly off-stoichiometry showed more complicated behavior.