Isothermal crystallization kinetics of amorphous Ga–Sb–Te films was studied by means of a time-resolved optical transmission method. Thin films with compositions along the pseudo-binary tie-lines Sb7Te3–GaSb and Sb2Te3–GaSb in the ternary phase diagram were prepared by the co-sputtering method. Crystallization of GaSbTe films reveals a two-stage process: an initial surface nucleation and coarsening (Stage 1) followed by the one-dimensional grain growth (Stage 2). The kinetic exponent (n) value in Stage 1 shows strong dependence on film compositions, while that of Stage 2 is less dependent. The activation energy in Stage 1 increases with increasing GaSb content and reaches the maximum values at compositions close to GaSb, but a decreasing trend was observed in Stage 2. Kinetics parameters between isothermal crystallization of thin films and non-isothermal crystallization of powder samples analyzed by differential scanning colorimetry [J. Mater. Res. 19, 2929 (2004)] are compared. The kinetic parameters in Stage 1 show much correspondence with those of non-isothermal cases in comparable kinetic exponents but with lower activation energies. The discrepancies between nonisothermal and isothermal kinetics are attributed to the sample morphology and the constraint effects.

A low-temperature (320–480 °C) metal-organic chemical vapor deposition (MOCVD) process was developed for the growth of ruthenium and ruthenium oxide thin films. The process used bis(ethylcyclopentadienyl)ruthenium [Ru(C5H4C2H5)2] and oxygen as, respectively, the ruthenium and oxygen sources. Systematic investigations of film formation mechanisms and associated rate limiting factors that control the nucleation and growth of the Ru and RuO2 phases led to the demonstration that the MOCVD process can be smoothly and reversibly modified to form either Ru or RuO2 through simple and straightforward modifications to the processing conditions–primarily oxygen flow and substrate temperature. In particular, films grown at low oxygen flows (50 sccm) exhibited a metallic Ru phase at processing temperatures below 480 °C. In contrast, films grown at high oxygen flow (300 sccm) were metallic Ru below 400 °C. Above 400 °C, a phase transition was observed from Ru to RuOx (0 < x < 2.0) to RuO2 as the processing temperature was gradually increased to 480 °C.

Ferroelectric layered perovskite SrBi2Nb2O9 has been successfully prepared through a new process using BiNbO4 as a precursor. The SrBi2Nb2O9 formation mechanism was investigated using a nonisothermal analysis method at constant heating rates. The weight loss recorded in thermal analysis under different heating rates was analogized to the reaction conversion. A combination of the differential and integral methods was introduced to solve the reaction mechanisms. Analysis using the differential method revealed that two kinds of diffusion-controlled models have higher linear correlation coefficients than other models. Based on the integral method principle, a new integral equation combining the Arrhenius equation and the Lobatto approximation was derived in this study. The established equation significantly simplified the conventional calculation process and improved the accuracy for predicting the reaction models. Analysis using the integral method corroborated that the SrBi2Nb2O9 formation mechanism is governed by Jander's diffusion controlled model, and the activation energy was calculated to be 192.1 kJ/mol. The proposed methods and the derived equations can be further applied to other solid-state-reaction systems to elucidate their reaction kinetics and estimate the related kinetic parameters.

Effects of loading rate and temperature on tensile behavior have been studied in air using two kinds of orthogonal three-dimensional woven Si–Ti–C–O fiber-reinforced Si–Ti–C–O matrix composites, processed by polymer infiltration and pyrolysis (PIP) and chemical vapor infiltration (CVI). Since the interphase and porosity of the two composites are controlled in as similar a manner as possible, the effect of matrix processing method is understood. The strength of the PIP composite is greater than that of the CVI composite at room temperature, but they are almost the same at high temperatures. It was found that the PIP composite is more sensitive to loading rate than the CVI composite due to more glassy phases in the PIP composite.

Microstructures and morphological features of a series of sintered quasicrystalline Al62.5−xCu25.3Fe12.2Bx alloys, with x ranging from 0 to 5 at.% were studied using x-ray diffraction, scanning electron microscopy, x-ray mapping, and electron probe microanalysis. Electron backscattering diffraction (EBSD) was also used to get information about the structures of some phases and identify the crystalline relationship in-between phases. Increasing x results in the change of the nature of extra phases. These secondary phases are all less than 1% in volume of the total matter except for the β phase at 5% of boron. Whatever the percentage of boron considered, boron seems to concentrate essentially in the parasite phases confirming doubts found in literature about the solubility of boron inside the face-centered-icosahedral Al–Cu–Fe phase. No special crystallographic relationship in between the tested phases could be spotted. EBSD is thus also confirmed as an excellent technique to get quasicrystalline grains orientations.

A new method of dynamic nanoindentation testing is introduced in this paper. Conventional dynamic nanoindentation testing involves the superposition of a single frequency sinusoidal force or displacement onto the quasi-static load–displacement curve. However, the viscoelastic response of many materials depends upon the frequency of the deformation of the material. This paper describes a method whereby the storage and loss modulus of viscoelastic solids can be determined using a multi-frequency dynamic oscillatory motion mode of deformation. In this method, the applied load is modulated by a pseudo-random force signal comprising multiple frequencies. A Fourier analysis is then used to deconvolute the signal into frequency-dependent values of storage and loss modulus for the specimen material as a function of frequency. The instrument response is cancelled by the use of a reference transfer function using an equalization process. Established modeling equations can then be used to extract the modulus of elasticity and the viscosity of the specimen material.

N-type nanocrystalline titania is a promising material for use in semiconductor photoelectrochemical cells and, potentially, the solar generation of hydrogen. In this study, we examined the photochemical properties of titania nanotube arrays made by anodization of a starting Ti foil in a fluoride ion containing electrolyte. The absorption properties of the titania nanotube samples were investigated using diffuse reflectance ultraviolet (UV)-visible (vis) spectroscopy, with a broadening of the absorption spectra seen as a function of material phase, nanotube diameter, and Pd sensitization. The magnitude of the anodic photocurrent obtained from the polycrystalline nanotube samples, measured under band gap UV illumination, appeared to be significantly higher than that reported for any other form of nanocrystalline titania. A maximum photoconversion efficiency (UV light exposure at 365 nm, intensity 146 mW/cm2) of 4.8% was obtained for 22 nm diameter nanotubes annealed at 500 °C and coated with a discontinuous palladium layer of 10 nm average effective thickness.

The static magnetic field and the alternating electric field were simultaneously imposed on AZ91D magnesium alloy melt, and α-dendrite particles were refined by the electromagnetic vibrations. The effect of the frequency of electromagnetic vibrations on microstructural refinement was quantitatively investigated. In the frequency range from 60 to 1000 Hz, the vibration frequency near 200 Hz was the most effective for the refinement of α-dendrite particles, and α-dendrite particles were refined up to approximately 100 μm from 1800 μm at this frequency. However, the effect of refinement by the electromagnetic vibrations became weak at frequencies above 400 Hz. Although the degree of refinement of the primary particles differed with the frequency of the electromagnetic vibrations, the dendrite arm spacing was almost constant, 30–40 μm, in our experiment. Therefore, the refinement of primary α-dendrite particles is likely to be caused by collapse of dendrite arms due to the cavitation phenomenon and the stirring of the melt.

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.

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.

The four-point bend (4PB) test is an industry standard in assessment of adhesion in thin films. Obtaining crack propagation along the desired interface plays a cardinal role in the success of this test. Crack penetration and deflection at a bimaterial interface has been extensively studied in the past. Most general results are based on asymptotic analyses involving the interface between two semi-infinite media. The results of these analyses cannot be directly used in case of the 4PB test since the boundary conditions and finite size effects in actual test specimen geometry are not accounted for. The purpose of this paper is twofold: first to develop a simple methodology to understand the preferred failure mode in a 4PB test and gain insight into the factors governing its success; second to examine the extent to which the results can be reconciled with those reported previously based on analysis of a crack in two semi-infinite media bonded together at the interface.

Advancements in nanotechnology for material processing via combustion synthesis have spurred the development of superalloys that provide improved protective properties. Nanoscale reactant particles offer unique thermal properties and increased homogeneity that improve the microstructural features and macroscopic properties of the synthesized product. In this study nanoscale molybdenum trioxide (MoO3) particles were added to micron scale nickel (Ni) and aluminum (Al). The goal was to incorporate a nanoscale additive within the reactant matrix that would produce a superalloy by generating excessively high heating rates and creating controlled quantities of Al2O3 (a strengthening agent) within the microstructure of the alloy. Ignition and flame propagation were examined using a CO2 laser and imaging diagnostics that include a copper-vapor laser coupled with a high-speed camera. Product microstructure was examined using micro-x-ray diffraction analysis and scanning electron microscopy. Abrasion testing was performed to evaluate the wear resistance properties of the superalloy. Results show that adding MoO3 increases the flame temperature, results in greater ignition sensitivity, produces a more homogeneous microstructure, and increases the overall wear resistance of the product.

A combustion synthesis method was developed for synthesis of AlN powder. Al powder and small amounts of urea were thoroughly mixed and placed in aluminum containers. A layer of AlN powder was placed on the top of the reactant powdersand in between the reactant powders and the container walls. The combustion reaction was ignited by heating the top surface of the powder stack and the aluminum container was converted completely to AlN during combustion reaction. High product yields (∼99.5%) were obtained under N2 pressures of 0.3–0.5 MPa. The product as synthesized is porous and loose and can be easily ground. A quenching technique was developed and formation of the various types of product morphology was investigated. Effects of several process parameters on the product yield were also studied. These results were reported and discussed.

The glass formability of high-manganese amorphous steel alloys reported earlier by us has been found to improve upon additions of yttrium and lanthanide elements, enabling the formation of bulk glassy samples with diameter thicknesses reaching 7 mm by casting. Based on extensive studies using different Ln additions and systematic measurements of alloy oxygen contents, the intrinsic roles of Y/Ln in attaining good glass formability in both the high-Mn alloys and previously reported high-Cr alloys are revealed. The yield strengths of the non-ferromagnetic glassy alloys obtained are estimated to be three times those of high-strength stainless steel alloys, and high elastic moduli in the range 150–200 GPa are measured. Furthermore, in the supercooled liquid regions, the glassy rods can be bent into various configurations by hand without fracturing. The observed plastic behavior together with the measured high mechanical strengths suggests that the present Fe–based bulk metallic glasses can potentially be developed as formable non-ferromagnetic amorphous steel alloys.

A semi-analytical approach was developed to study the creep response of a viscoelastic polymeric thin film on a hard elastic substrate under flat-ended punch indentation. This approach allows one to separate mechanical properties of the film from its substrate. To verify the approach, flat-ended punch creep indentation tests were performed to obtain the long-time viscoelastic behaviors of a polymethyl-methacrylide film overlying on an aluminum substrate. Three viscoelastic models describing the constitutive equations of the polymer film are compared in this paper. “Film-only” viscoelastic parameters were extracted by fitting with the experimental creep curves of flat-ended punch indentation. It is shown that the present approach provides an effective way to characterize the mechanical properties of a polymeric film on an elastic substrate.

When exposed to air at room temperature, Zn nanoparticles oxidize gradually to form crystalline ZnO shells with a thickness of a few nanometers. Electron diffraction and high-resolution lattice imaging revealed that the ZnO layer on the Zn {0001} surface is composed of many epitaxial domains with small rotation angles relative to the lattice of the Zn core. The oxidized Zn particle bends when irradiated by the electron beam in a transmission electron microscope. This is due to the increase of internal stress in the ZnO layer as a result of the realignment of adjacent domains under electron beam irradiation. Corrosion of Zn nanoparticles was observed and the scaling and spalling start to occur on the {1010} prismatic faces.

An analytical solution for shape evolution of a coherent misfit precipitate in triaxially stressed solid has been proposed based on Eshelby inclusion theory. With complete energy consideration, the free energy that controls the shape evolution of the precipitate is a function of the precipitate shape, size, triaxially applied stresses, misfit strains, and Young’s moduli of the precipitate and the matrix. Based on the energy analysis, a comprehensive picture of shape evolution of the precipitate is presented.

Simple equations are proposed for determining elastic modulus and hardness properties of thin films on substrates from nanoindentation experiments. An empirical formulation relates the modulus E and hardness H of the film/substrate bilayer to corresponding material properties of the constituent materials via a power-law relation. Geometrical dependence of E and H is wholly contained in the power-law exponents, expressed here as sigmoidal functions of indenter penetration relative to film thickness. The formulation may be inverted to enable deconvolution of film properties from data on the film/substrate bilayers. Berkovich nanoindentation data for dense oxide and nitride films on silicon substrates are used to validate the equations and to demonstrate the film property deconvolution. Additional data for less dense nitride films are used to illustrate the extent to which film properties may depend on the method of fabrication.

This paper describes the growth kinetics of an interfacial MgO layer as well as those of an MgB2 layer during ex situ annealing of the evaporated amorphous boron (a-B) film under Mg vapor overpressure. A thin MgO layer is formed at the interface between a-B and Al2O3 substrate before the formation of crystalline MgB2 layer and the interfacial layer is epitaxially related with Al2O3 substrate (MgO (111)[110] // Al2O3 (0001)[1100]). The interfacial MgO layer continues to grow during the annealing, and its apparent growth rate is about 0.1 nm/min. The analysis of MgB2 layer growth kinetics using cross-sectional transmission electron microscopy reveals that there exist two distinct growth fronts at both sides of an MgB2 layer. The growth kinetics of the lower MgB2 layer obeys the parabolic rate law during the entire annealing time. The growth of the upper MgB2 layer is controlled by the surface reaction between out-diffused boron and Mg vapor up to 10 min, resulting in a rough surface morphology of MgB2 layer. By considering the mass balance of Mg and boron during ex situ annealing, we obtained the diffusivities of Mg and boron in MgB2 layer which were in the same order range of approximately 10−12 cm2/s.

A detailed study of the size, distribution, and morphology of oxide particles in as-sprayed deposited 5083 Al synthesized by reactive atomization and deposition was reported. The results indicated that the oxides exhibit thin-plate morphology and are distributed at prior droplet boundaries, grain boundaries, and grain interiors with a dimensional scale on the order of tenths of micrometers up to a few micrometers. The mechanisms involved in the formation of the observed oxide distribution were analyzed in detail.