The fabrication and applications of porous anodic alumina (PAA) have been studied for decades. Recently, preparation of PAA template directly formed on Si has been developed to enhance the performance of the fabricated nanostructures. However, less attention is paid to the anodization mechanism of the Al film on the Si substrate. In the current study, the PAA template was fabricated on Si of which an interlayer was sandwiched between the Al film and the Si substrate. The anodization behavior of the Al film, especially at the alumina–substrate interface, was investigated through the observation of the variation of oxidation current and the structural change of alumina. Different degree of dissolution at the pore base of alumina was revealed when a different interlayer was introduced, leading to the formation of the arched pore bottom. At the same time, difference in the variation of current was also observed as the pore base reached the alumina–Si interface. These features were different from those observed in conventional anodization of Al foils. The findings in this study are of scientific and technological importance for the template-mediated growth of nanostructures, especially for those to be integrated into Si devices.

Nanostructured Ti5Si3–TiC–Ti3SiC2 and Ti5Si3–TiC composites were in situfabricated through the spark plasma sintering (SPS) technique using Ti and SiC powders as reactants. It was found that the composites could be prepared in arelatively short time (6 min at 1260 °C) above 98% theoretical density. The phase constituents and microstructures of the samples were analyzed by x-ray diffractionand observed by scanning electron microscopy. Transmission electron microscopywas used for detailed microstructural analysis. The results showed that the reaction products mainly consisted of Ti5Si3 and TiC phases or Ti5Si3, TiC and Ti3SiC2phases, depending on the molar ratio of reactants (Ti to SiC). The composites exhibited fine microstructure; TiC grain size was less than 200 nm. Fracturetoughness at room temperature was also measured by indentation tests.

Carbon nanotubes have been synthesized by chemical vapor deposition using a thin iron film as catalyst on the silicon substrate with different-sized rectangular patterns. It is found that the carbon nanotubes grow vertically to the substrate in a high density with a surface shape similar to that of the substrate when the line width of the patterns are larger than 1 μm, However, when the line width of the pattern is reduced to below 0.5 μm, carbon nanotubes cannot grow vertically anymore. This phenomenon might be caused by the relaxation of stress in catalyst film and the coalescence of the catalyst clusters to form particles or grains, which contributes to the migration of catalyst from edge to inner part during the nucleation process. These results are very useful for the fabrication of field-emission displays and other devices using patterned carbon nanotubes.

Several thermophysical properties of liquid and supercooled ruthenium were measured using electrostatic levitation. Over the 2225–2775 K temperature interval, the density can be expressed as ρ(T) = 10.75 × 103 – 0.56(T – Tm)(kg ⋅ m−3) with Tm = 2607 K. In addition, the surface tension can be expressed as σ(T) = 2.26 × 103 – 0.24(T – Tm)(mN ⋅ m−1) and the viscosity as η(T) = 0.60 exp[4.98 × 104/(RT)] (mPa ⋅ s) over the 2450–2725 K range. The isobaric heat capacity was estimated as CP(T) = 35.9 + 1.1 × 10−3(T – Tm)[(J/(mol K)] over the 2200–2750 K span by assuming a constant emissivity. The volume expansion coefficient, the enthalpy, and the entropy of fusion were also calculated as 5.2 × 10−5 K−1, 29.2 kJ ⋅ mol−1, and 11.2 J/(mol K).

Both analysis and numerical calculations have been carried out to investigate the relationship between Young’s modulus and nonideally sharp indentation parameters. The results confirm that there exists an approximate one-to-one correspondence between the ratio of nominal hardness/reduced Young’s modulus (Hn/Er) and the ratio of elastic work/total work (We/W) for any definite bluntness ratio (Δh/hm) of a nonideally sharp indenter. Based on this relationship, the Young’s modulus of the indented material can be determined just from the values of Hn, We, and W, which are directly measurable quantities in an indentation test.

Single crystalline nanorods (15–200 nm in diameter and hundreds nanometers in length) have been formed on the carbon-covered W wires by simple electric heating under a vacuum of 5 × 10−4 Pa. The chemical composition and crystalline structure of the nanorods were carefully investigated by various characterization techniques such as scanning electron microscopy, transmission electron microscopy, Raman spectroscopy, energy dispersive x-ray spectroscopy and electron energy loss spectroscopy. After ruling out any possible existence of carbon nanotubes (CNTs), tungsten carbide, W–Fe alloying, and formation of other types of tungsten oxides, monoclinic W18O49 phase has been well identified. The mechanism of nanorod formation of sub-tungsten oxide (∼WO2.7 compared to WO3) will be discussed in relation to the sample preparation conditions.

Europium-doped lutetium oxide (Lu2O3:Eu3+) nanophosphors were synthesized via modified combustion technique using urea as the fuel and metal nitrates as oxidants. The pellets prepared from the calcined nanocrystalline powders were vacuum sintered up to 1750 °C leading to very translucent ceramic. The products were characterized by x-ray diffraction to ascertain phase purity. The microstructures reveal the nanocrystalline nature of the powders. We have illustrated the crystallite size dependence and the influence of Eu3+ activation of Lu2O3:Eu3+ nanophosphors on Raman scattering. We have also demonstrated the particle size dependence of emission characteristics of nanophosphors and ceramics. Our results suggest that although the processed ceramics display superior emission characteristics, the nanocrystalline phosphor powders calcined at 1100 °C also display reasonably good emission characteristics, illustrating the possibility of their applications in display technology.

Elastic modulus of bone was investigated by nanoindentation using common methods of sample preparation, data collection, and analysis, and compared to dynamic mechanical analysis (DMA: three-point bending) for the same samples. Nanoindentation (Berkovich, 5 μm and 21 μm radii spherical indenters) and DMA were performed on eight wet and dehydrated (100% ethanol), machined equine cortical bone beams. Samples were embedded in polymethylmethacrylate (PMMA) and mechanical tests repeated. Indentation direction was transverse to the bone long axis while DMA tested longitudinally, giving approximately 12% greater modulus in DMA. For wet samples, nanoindentation with spherical indenters revealed a low modulus surface layer. Estimates of the volume of material contributing to elastic modulus measurement showed that the surface layer influences the measured modulus at low loads. Consistent results were obtained for embedded tissue regardless of indenter geometry, provided appropriate methods and analysis were used. Modulus increased for nanoindentation (21 μm radius indenter) from 11.7 GPa ± 1.7 to 15.0 GPa ± 2.2 to 19.4 GPa ± 2.1, for wet, dehydrated in ethanol, and embedded conditions, respectively. The large increases in elastic modulus caused by replacing water with ethanol and ethanol with PMMA demonstrate that the role of water in fine pore space and its interaction with collagen strongly influence the mechanical behavior of the tissue.

The kinetics of methanol transport in 2-hydroxyethyl methacrylate (HEMA) homopolymer and 75/25 and 50/50 mol fraction HEMA/DHPMA (2,3-dihydroxypropyl methacrylate) copolymers at five different temperatures has been investigated using the sorption experiment technique. A combined case I and case II diffusion model was used to describe the transport processes. Four replicates for each temperature of each material having a nominal thickness of 0.1 mm were immersed in methanol maintained at 35, 40, 45, 50, and 55 °C, and the mass uptake as a function of time was measured gravimetrically. Experimental results are found to be in good agreement with model prediction at all temperatures and for all three materials. Both the diffusion coefficients of case I transport and velocity of case II transport increase with increasing temperature. D values at low temperatures (35 and 40 °C), which are in the 10−9 cm2/s range, of the HEMA homopolymer are less than those of the copolymers. On the other hand, the activation energies of case I transport of the copolymers are substantially higher than those of the HEMA homopolymer; however, the level of DHPMA loading in the copolymer does not seem to affect the activation energy. In addition, thermodynamic heat and free energy of mixing values indicate heat is released when HEMA/DHPMA copolymers are exposed to methanol and that the solvent/copolymer systems exist as a continuous phase. In contrast, the methanol/HEMA homopolymer system exists as separate phases.

We developed an Al2O3 and Al3Ni intermetallic reinforced Al-based metal matrix composite by sintering an Al-20 wt% NiO powder compact at 1000 °C. Differential thermal analysis showed that a two-step reaction took place between Al and NiO in the temperature range 600–650 °C. The initial stage was a solid-state reaction, but it was soon paused by the newly formed Al2O3 and Al3Ni phases that separated the Al and NiO grains. A liquid–solid reaction was later resumed as the temperature was increased above the eutectic temperature of Al–Al3Ni at 640 °C when molten Al–Ni appeared. When the molten sample was quenched to room temperature, a two-phase Al–Al3Ni eutectic was found in the sample. In comparison with the air-quenched and the oil-quenched samples, the sizes of proeutectic Al3Ni grains and Al–Al3Ni eutectic phases in the salt-solution-quenched sample were much finer. The eutectic contained Al3Ni nanofibers with a diameter of approximately 50 nm. A reaction model of Al and NiO was proposed. A thermodynamic model was also proposed to describe the formation of the composite.

Depth-sensing indentation was applied to three-dimensionally ordered silica foams of two different pore diameters—500 nm and 850 nm—formed by colloidal crystal templating. The contact responses of indentations with Berkovich and hemispherical indentation tips are presented over a load range of 1 mN to 100 mN. Scanning electron microscopy images of residual indentation impressions showed homogeneous deformation for small loads in which the peak displacement was shallow relative to the film–substrate interface. The characteristics of the load–displacement responses changed from periodic discontinuities, associated with cell wall fracture and pore collapse, to smooth and increased stiffness, as a result of densification due to the accumulation of material under the indentation tip and proximity (and contact) of the substrate. Load–displacement responses were translated into pressure–volume space, in which the average pressure during indentation is a measure of the crushing pressure of the cell walls.

We propose a nucleation theory-based analysis for incipient plasticity during nanoindentation and predict the statistical distribution of rate-dependent pop-in events for many nominally identical indentations on the same surface. In the framework of stress-assisted, thermally activated defect nucleation, we quantitatively rationalize new nanoindentation measurements on 4H SiC and extract the activation volume of the nucleation events that mark the onset of plastic flow. We also illustrate how this statistical approach can differentiate between unique nucleation events for different indenter tip geometries.

Growth behavior and microstructure of oxide scale formed on MoSi2 coating by cyclic oxidation testing in air at 500 °C were investigated using field emission scanning electron microscopy, cross-sectional transmission electron microscopy, glancing angle x-ray diffraction, and x-ray photoelectron spectroscopy. MoSi2 coating was prepared by chemical vapor deposition of Si on a Mo substrate at 1100 °C for 5 h using SiCl4–H2 precursor gas mixtures. After the incubation period of about 454 cycles, accelerated oxidation behavior was observed in MoSi2 coating and the weight gain increased linearly with increasing oxidation cycles. Microstructural analyses revealed that pest oxide scale was formed in three sequential processes. Initially, nanometer-sized crystalline Mo4O11 particles were formed with an amorphous SiO2 matrix at MoSi2 interface region. Inward diffusing oxygen reacted with Mo4O11 to form Mo9O26 nano-sized particles. At final stage of oxidation, MoO3 was formed from Mo9O26 with oxygen and growth of MoO3 took place forming massive precipitates with irregular and wavy shapes. The internal stress caused by the growth of massive MoO3 precipitates and the volatilization of MoO3 was attributed to the formation of many lateral cracks into the matrix leading to pest oxidation of MoSi2 coating.

Nanocrystalline boehmite obtained by limited hydrolysis of aluminum tri-sec-butoxide or aluminum chloride was aged under different conditions before being calcined above the dehydroxylation temperature. When aging was carried out under hydrothermal conditions, the condensation of the structural units obeyed a first-order kinetic law with apparent activation energy of 12.2 kcal/mol. Under dehydroxylation conditions, the boehmite fragmentation is accounted for by a simple power law that links its volume to that of the resulting γ-alumina. The main variable is the volatile compounds content (water for instance) in the fresh sample. In terms of texture, a better organization of the initial nanoparticles in the boehmite means a lower surface area and larger pore diameter in the corresponding γ-alumina.

Highly oriented Pb(Zr,Ti)O3 (PZT) films were deposited on Pt/Ti/SiO2/Si substrates by the sol-gel method using lanthanum nitrate as a buffer layer. When the lanthanum nitrate buffer layer was heat treated at temperatures between 450 and 550 °C, the PZT layer coated onto this buffer layer showed a strong (100) preferred orientation. Regardless of the other deposition conditions, such as the pyrolysis temperature, pyrolysis time, annealing temperature and heating rate, the film deposited on the buffer layer had this orientation. Thick films were also fabricated using the sol-gel multi-coating method, and the (100) texture was found to be maintained up to a thickness of 10 μm. The ferroelectric hysteresis and piezoelectric coefficient (d33) of highly oriented PZT thick films were characterized, and the (100) oriented PZT film showed higher piezoelectric property than the (111) oriented film.

The microwave irradiation technique (MWIT) was applied to synthesize lithium manganese oxide having spinel structure using LiOH·H2O and ε–MnO2 as starting materials. The crystal and electronic structure depends on the irradiation time; x-ray diffraction patterns of the sample irradiated for 9 min were in good agreement with that of cubic structure without showing the peak of MnO2. The electronic structure of synthesized samples before and after lithium ion intercalation and/or deintercalation was investigated by Mn L-edge and O K-edge x-ray absorption spectroscopy.

An approach to pattern directly thin films of various materials deposited by different physical vapor deposition methods is presented. Co and Ag films deposited by pulsed laser deposition and e-beam evaporation, respectively, were fabricated into 650- and 1000-nm-spaced parallel stripes on Si(100) surfaces by simultaneous two-beam ultraviolet laser interference irradiation of the substrate surface during deposition. The resulting morphology consists of 1- to 2-nm-height stripes, which have the same direction and spacing as the interference fringes. This approach has the potential to allow long-range ordering of well-defined patterns over large areas because the spacing and geometrical patterns are defined by the laser interference. Furthermore, the fact that this method works for different materials and does not require any lithography masks, etching steps, or substrate prepatterning, makes it promising as a simple and economical lateral patterning approach.

In the Sn–9Zn–xAg (x ranges from 0.5 to 3.0%) solder system, the Ag–Zn intermetallics start crystallizing as β–AgZn at about 300 °C. Subsequently, the solder experiences two peritectic transformations upon solidification. This results in the multiphase structural feature. The complicated crystallization process can be briefly described as L(liquid) → L + AgZn → L + AgZn + Ag5Zn8 → AgZn + Ag5Zn8 + AgZn3.

The effect of ZrO2–3 mol/ Y2O3 sol-gel thin coatings on the fracture of soda-lime glass is investigated. For this purpose, a recently developed strength measurement procedure—based on making a brittle material flex on top of a soft substrate by applying a load with a spherical indenter to the top surface of the system—is used. Results suggest significant variation of both the average fracture strength and the Weibull modulus on coated glass slides. It is suggested that the origin of such variations can be attributed to a certain chemical degradation of the glass during the coating process. This chemical attack produces a highly homogeneous flaw population on the glass surface which governs its fracture behavior. Implications of this work for the practical use of coated glass layers are discussed.

Sol-gel materials of aluminum-modified TiO2 of nominal composition 5.7 wt% and 10.8 wt% aluminum and aluminum/vanadium co-modified TiO2 of nominal composition 5.7Al–3.5V wt% have been prepared by evaporation of aqueous colloidal sols obtained by the hydrolysis of aqueous solutions of titanium chloride with the appropriate amount of vanadyl oxalate and/or aqueous aluminum nitrate using aqueous ammonia followed by peptization of the resulting hydrated solids using nitric acid. The nature of the sol-gel materials and the behavior upon calcination at temperatures up to 1373 K have been investigated using x-ray fluorescence, x-ray powder diffraction, transmission electron microscopy, and electron diffraction. At 333 K, all the gels comprise small (approximately 5 ± 1 nm) particles of anatase together with traces of brookite and highly crystalline ammonium nitrate. The particle size changes little on thermal treatment at 573 K, but increases significantly at higher temperatures and is accompanied by transformation to rutile. Aluminum-modified gels stabilize the anatase phase from 923 K in unmodified TiO2 to 1023 K in the 6Al/TiO2 gel and 1173 K in the 11Al/TiO2 gel. The alumina in the co-modified gel has a dominating effect on stabilizing the anatase phase until 973 K. Only rutile is present at high temperatures, except for small amounts of phase-separated α-Al2O3 (Corundum). No substitutional incorporation of Al3+ ions in the tetragonal rutile lattice occurs at high temperatures.