A study comparing the morphology and electrical transport properties of pentacene films on underlayers of different self-assembled monolayers (SAMs) is presented. The SAMs studied as underlayers were phenyltrichlorosilane, n-octadecyltrichlorosilane, and t-butyldiphenylchlorosilane. Pentacene thin films were grown by vacuum sublimation on SiO2 surfaces treated with self-assembled monolayers. During deposition, substrates were held at a temperature of 70 °C. The morphologies of the films at different stages of deposition were studied by atomic force microscopy, and the transport properties of the films were characterized by I-V measurements in a simple field-effect transistor (FET) structure. The SAM underlayers strongly influence the film morphology in the first few molecular layers and hence significantly impact the electrical transport in the resulting FETs.

Nanocrystalline tungsten oxide (WO3) films were electrodeposited potentiostatically at room temperature on transparent conducting substrates from an ethanolic solution of acetylated peroxotungstic acid prepared from a wet chemistry process. The changes that occur in the microstructure and the grain size of the as-deposited WO3 films as a function of annealing temperature are simultaneously accompanied by a continually varying electrochromic performance. X-ray diffraction studies revealed the transformation of a nanocrystalline as-deposited WO3 film into a highly crystalline triclinic WO3 as the annealing temperature was raised from room temperature to 500 °C. The microstructural evolution with the increasing annealing temperature of the as-deposited film was further exemplified by transmission electron microscopy (TEM) studies. While the as-deposited film was composed of uniformly distributed ultra fine nanograins, the most noticeable feature seen in these films annealed at 250 °C was the presence of open channels which are believed to promote lithium ion motion. Films annealed at 400 °C exhibited coarse grains with prominent grain boundaries that hinder lithium ion movement, which in turn reduces the film’s ion insertion capacity. In concordance with the TEM results, the 250 °C film had the highest ion storage capacity as it exhibited a charge density of 67.4 mC cm−2 μm−1. The effect of microstructure was also reflected in the high transmission modulation (64%) and coloration efficiency (118 cm2 C−1) of the 250 °C film at 632.8 nm. Contrary to the superior electrochromic performance of the 250 °C film, the optical switching speeds between the colored and bleached states of the as-deposited WO3 film declined considerably as a function of annealing temperature. Also, the diffusion coefficient for lithium ions was greater by at least an order of magnitude for the as-deposited film as compared to the 250 and 500 °C films. In this report, the influence of microstructural changes that are brought about by the annealing of the as-deposited WO3 films on their coloration-bleaching dynamics is evaluated in terms of their structural, electrochromic, and electrochemical properties.

Ti1−XSbXO2 samples were obtained from dip-coating sol-gel method and a subsequent anneal at 450 °C. They had an average crystallite size of 13.3–20 nm. Cyclic voltammograms taken under ultraviolet (UV) and Xe lamp illumination in a 0.5 M Na2SO4 electrolyte showed that the Sb-doped samples had greater photocurrent densities than pure titania electrode, with an optimal Sb concentration of 0.2%. Oxidative peaks were observed in the cyclic voltammograms obtained in the dark after certain exposure duration to UV light. X-ray diffraction patterns and Raman spectra show a phase transformation from brookite to anatase in the samples with Sb concentration up to 0.2%. Ti4+ ions were substituted by Sb to form the anatase structure of Sb–O–Ti, improving the crystallization efficiency. The Sb–Sb bonds were formed due to the introduction of excessive Sb atoms.

A method for preparing rare-earth element-doped yttrium oxide phosphor photonic band gap crystals (PBG) is described, which obviates the necessity for multiple infilling of the opal-like template. The method utilizes (i) the re-dissolving and the concentration of previously precipitated spherical phosphor particles made by homogeneous precipitation methods into a viscous precursor phosphor solution, and (ii) formation of an opal-like template of polystyrene or silica spheres. A procedure is outlined that permits the precursor solution to be drawn into the template in a controlled manner that can be easily monitored using an optical microscope. Attenuation of the strong, red cathodoluminescent emission is observed in Y2O3:Eu3+ phosphor PBG crystals that are engineered to have a stopband overlapping the emission bands in the red region. This attenuation results from Bragg diffraction of the light emitted within the PBG phosphor crystals.

The converse piezoelectric response of a thin film constrained by a substrate is analyzed in different geometries under various boundary conditions. We considerthe effects of elastic deformation of the substrate on the total displacement of thefilm surface induced by the electric field. The change of film thickness and the bending curvature of a film/substrate couple are calculated. For a thin film island clamped on a large thick substrate, the theoretical estimation of the piezoresponse, including a local bending in the vicinity of the island/substrate interface, is in agreement with the finite element calculation.

Pt thin films of various thicknesses (30 nm ∼ 200 nm) were deposited on Si wafers with SiO2, Ti, TiO2, or IrO2 buffer layers at various temperatures (room temperature ∼200 °C) by a direct current magnetron sputtering process. The Pt films showed a strong (111)-preferred texture irrespective of the thickness, under-layer, and growth temperature. The authors previously reported [J-E. Lim, D-Y. Park, J.K. Jeong, G. Darlinski, H.J. Kim, and C.S. Hwang, Appl. Phys. Lett. 81, 3224 (2002)] that the films were composed of three kinds of grains with slightly different (111) lattice parameters (bulklike, 1.0% and 2.1% larger). This study details the microstructural variations of the Pt films according to the variations of experimental parameters. The different deposition conditions produced slightly different crystalline structures, but the three different (111) lattice parameters were always found. Epitaxial (200) Pt films on a (200) MgO substrate and a highly (111) textured Au thin film on a SiO2/Si did not show the same splitting in the lattice parameter. The grains with 1.0% and 2.1% larger (111) lattice parameter almost disappeared after postannealing at 1000 °C. However, surface chemical binding of the Pt film before and after annealing was unchanged. Therefore, it is believed that the lattice parameter splitting in the (111) textured Pt film originated from the interfacial grains with the distorted crystal structure due probably to growth stress.

The present work focuses on the severe plastic deformation and deformation twinning of 316L austenitic stainless steel deformed at high temperatures (700 and 800 °C) using equal channel angular extrusion (ECAE). Very high tensile and compressive strength levels were obtained after ECAE without sacrificing toughness with relation to microstructural refinement and deformation twinning. The occurrence of deformation twinning at such high temperatures was attributed to the effect of high stress levels on the partial dislocation separation, i.e., effective stacking fault energy. High stress levels were ascribed to the combined effect of dynamic strain aging, high strain levels (∈ ∼ 1.16) and relatively high strain rate (2 s−1). At 800 °C, dynamic recovery and recrystallization took place locally leading to grains with fewer dislocation density and recrystallized grains, which in turn led to lower room temperature flow strengths than those from the samples processed at 700 °C but higher strain hardening rates. Apparent tension-compression asymmetry in the 700 °C sample was found to be the consequence of the directional internal stresses.

Dense aluminum nitride ceramics were prepared by sintering green bodies at 1750 °C for 2 h. These green bodies were prepared by aqueous slip-casting from a powder that was surface-treated to prevent hydrolysis. The surface treatment of the aluminum nitride (AlN) powder consisted of dispersing the powder in warm-water solutions of aluminum dihydrogenphosphate Al(H2PO4)3. Different treatment temperatures in the range 30–80 °C were tested. For all the tested temperatures, the surface-treated AlN powder was found to be water-resistant, even after drying and/or redispersion. Various commercial dispersants were tested for their effectiveness, and the amount of dispersant was optimized in terms of a high solids loading of the suspension and an acceptable viscosity for slip casting. Based on these studies, a stable aqueous suspension of AlN powder, treated at 60 °C, with a total solids loading of 50 vol%, was prepared using CaF2 as a sintering additive. The well-dispersed powder made it possible to prepare green samples with close particle packing and relatively high sintered densities; that is, more than 96% of the theoretical density.

We have studied PET/0.6 PHB, an alternating copolymer in which PET is poly(ethylene terephthalate) and PHB is p-hydroxybenzoic acid with the mole fraction of 0.6 PHB. It is a longitudinal polymer liquid crystal (PLC) with the LC sequences in the main chain and oriented along the chain backbone. Material not subjected to the magnetic field, specimens oriented along and perpendicularly to the flux of the magnetic field, were investigated. Static friction, dynamic friction, scratch penetration depth, and healing of the material were determined. Static and dynamic friction parameters for oriented samples have significant higher values for oriented samples. The best scratch resistance is found for the sample aligned along the magnetic field. The results are explained in terms of morphology revealed by scanning electron microscopy and phase structures.

An analytical model was developed to derive an approximate closed-form solution for indenter displacement when a rigid spherical indenter is pressed onto a coating/substrate system. Finite element analyses were also performed to verify the analytical solution. The results showed that the solution could be obtained from the analytical expression for Hertzian indentation on a homogeneous semi-infinite elastic medium multiplied by a modification term. This modification term is a function of two ratios: (i) Young’s modulus ratio between the coating and the substrate and (ii) the ratio between the coating thickness and the contact radius. Based on this modification term, master curves for Hertzian indentation on coating/substrate systems were plotted.

The use of boron as a sintering aid reduces the sintering temperature, enhances the sintering density, and improves the microwave properties of Ba(Cd1/3Ta2/3)O3 ceramic dielectrics. Observations by transmission electron microscopy indicate that the liquid sintering mechanism contributes to the improvement in sintering density for boron concentrations exceeding 0.5 wt%. The introduction of as small as 0.01% boron also results in the production of high-density samples (∼95%), presumably indicating that a point defect mechanism may also play an important role in the sintering process. X-ray diffraction data combined with high-resolution transmission electron microscopy images show that boron-doped Ba(Cd1/3Ta2/3)O3 ceramic material has a well-ordered hexagonal structure. Annealing treatment is found to improve the microwave properties. The best sample has a dielectric constant of 32, a temperature coefficient of resonant frequency of 80 ± 15 ppm/°C, and a quality factor of >25,000 at 2 GHz.

A novel method was developed to produce Al2O3/AlN composite powders. The composite powders were synthesized by the direct nitridation of Al2O3 using various additives by plasma processed with two different types of gas (Ar/N2 and N2 plasma). The effects of these two different plasma gases and additives on the formation of the Al2O3/AlN composites were studied. The x-ray diffraction results in the composite powders showed that the cubic AlN was converted to the major phase while transient γ–Al2O3 was the minor phase when the composite powder was fully melted using nitrogen as the sole working gas. In contrast, the main phase was still α–Al2O3 when the composite powder was not well melted using the mixture of argon and nitrogen as the working gas. Carbon was found as an effective conversion additive to increase the cubic AlN of this composite powder up to 49 vol%. The reaction mechanism of forming this composite powder was also analyzed.

This study used an analytical model for phase-transformation kinetics. We used different combinations of various nucleation mechanisms [mixed nucleation (site saturation plus continuous nucleation), Avrami nucleation, and site saturation plus Avrami nucleation] and growth mechanisms (volume diffusion-controlled growth and interface-controlled growth) for a single transformation. Our work incorporated the effect of impingement of the growing particles. These factors have been applied to the same experimental results to find out the prevailing mechanisms. We made a detailed analysis for the determination of the parameters of the analytical phase-transformation model, in order to determine the most reasonable nucleation and growth modes, and the values for the activation energies of nucleation and growth. We used the model to study the crystallization kinetics of Mg82Ni18 and Mg88.7Ni11.3, as measured by means of both isothermal and isochronal differential scanning calorimetry.

In this paper a new loading history for extracting the stress–strain curve as well as the viscosity and creep behavior from indentation experiments is developed. It is based on a simple model describing the viscoplastic spherical indentation with a power-law hardening rule and a velocity-dependent overstress. Using this model, patterns were generated consisting of load-depth data and corresponding material parameters. The loading history for the simulation of the patterns was considered as a variable combination of loading and creep processes. To compare the identification potential of different loading histories, the inverse problem of determining the viscoplastic material parameters was solved by using neural networks. The emerging loading history uses a multiple-creep process with equidistant load steps and allows an identification of material parameters with much higher accuracy than with single creep. It will be used for further work, where the identification method is generalized using more realistic finite element simulations for a finite deformation elastic–viscoplastic material behavior.

Thin films of perfluorinated vanadyl phthalocyanine F16PcVO were prepared by physical vapor deposition in high vacuum on KBr and fused silica substrates. The absorption spectra in the visible region show that the films on different substrates have different structure. The optical constants for F16PcVO films were obtained in the spectral range of 0.7–4.5 eV from the simulation of ellipsometry spectra with an anisotropic uniaxial model. From the difference between the in-plane and out-of-plane components of the extinction coefficient the average tilt angle of the F16PcVO molecular planes with respect to the substrate plane was found to be 56° for fused silica substrates and between 0° and 3° for KBr substrates.

About 1.5-μm-thick single-layer TiN, CrN, TiAlN coatings and nanolayered TiN/CrN, TiAlN/CrN multilayer coatings were deposited on silicon (111) substrates using a reactive direct current magnetron sputtering process. Structural characterization of the coatings was done using x-ray diffraction (XRD) and micro-Raman spectroscopy. All the coatings exhibited NaCl B1 structure in the XRD data. Raman spectroscopy data of as-deposited coatings exhibited two broad bands centered at 230–250 and 540–630 cm-1. These bands have been assigned to acoustical and optical phonon modes, respectively. Thermal stability of the coatings was studied by heating the coatings in air in a resistive furnace for 30 min in the temperature range 400–900 °C. Structural changes as a result of heating were characterized using Raman spectroscopy and XRD. Raman data showed that TiN, CrN, TiN/CrN, TiAlN, and TiAlN/CrN coatings started to oxidize at 500, 600, 750, 800, and 900 °C, respectively. To isolate the oxidation-induced spectral changes as a result of heating of the coatings in air, samples were also annealed in vacuum at 800 °C under similar conditions. The Raman data of vacuum-annealed coatings showed no phase transformation, and intensity of the optical phonon mode increased and shifted to lower frequencies. The origin of these spectral changes is discussed in terms of defect structure of the coatings. Our results indicate that the thermal stability of nanolayered multilayer coatings is superior to the single-layer coatings.

The purpose of this research is to investigate the feasibility of the synthesis of platinum/multi-wall carbon nanotube (Pt/MWNT) catalysts and such catalysts' application in fuel cells. The as-received MWNTs were purified and decorated by pretreatment. Infrared-spectrum indicates the carboxylic (-COOH) and carbonyl (-C=O) groups were introduced on the surface of the MWNTs after pretreatment. These functional groups will act as anchor sites for the Pt deposition. Then the Pt particles in nano scale were deposited on the surface of MWNTs by reduction of a solution of hexachloroplatinic acid. Transmission electron microscopy examination reveals that Pt particles are attached to the surface of MWNTs. If as-received MWNTs are not pretreated in the proper way, the Pt particle aggregates are mostly found on the open end of MWNTs. Occasionally Pt penetrated inside the tube of MWNTs. The relationship between the Pt particle morphology and the conditions of pretreatment and reduction reaction is discussed. After heat treatment, Pt particles recrystallized to form the Pt/MWNT catalysts. The Pt/MWNT catalysts were applied to a single cell and the test result shows a promising future of these catalysts with low Pt loading when applied in proton exchange membrane fuel cells (PEMFCs).

Thin films of vanadium oxides were grown on fused quartz by metalorganic chemical vapor deposition using vanadyl acetylacetonate as the precursor. Growth at temperatures ⩾560 °C results in composites of strongly (00l)-oriented V2O5 and V6O13. The dominant phase of the film changes from V2O5 to V6O13, and back to V2O5, as the growth temperature is raised from 560 to 570 °C, then to 580 °C, as evidenced by x-ray diffraction and Rutherford backscattering analyses. This reentrant-type growth trend was interpreted on the basis of the small difference in the free energy of formation of V2O5 and V6O13 and the presence of metal–oxygen bonds in the precursor. In contrast with single-crystalline V6O13, the film predominantly composed of highly oriented single-crystalline platelets of V6O13 did not undergo the semiconductor–metal transition at −123° K, despite the connectivity being well above the percolation threshold. Instead, a semiconductor-to-semiconductor transition was observed in this film, which is explained in terms of the observed relaxation of the edges of all the platelets of metallic V6O13 to semiconducting V2O5.

The effect of nanoscale Pt particles embedded in ferroelectric matrix on the polarization switching characteristics of Pb(Zr0.5Ti0.5)O3 (PZT) thin films of low thickness was investigated. Two different nanocomposite structures of PZT-Pt thin films were fabricated for the study. The first one incorporated a single layer of Pt nano-particles embedded in the PZT film, which was formed by annealing an ultrathin Pt layer that had been inserted into the middle of the deposited PZT. The other one had Pt nano-particles embedded uniformly and coherently in the lattice of the PZT matrix, which was generated by annealing the cosputtered films of PZT and Pt. The electric field applied on the films can be locally intensified near the embedded Pt particles, which markedly enhances the polarization switching characteristic of the above PZT-Pt nanocomposite films. Accordingly, a satisfactorily higher remanent polarization was obtained than exhibited by normal PZT films, but the coercive field was only slightly higher. However, adding an excess of Pt made the nanocomposite films too leaky to exhibit the enhancement. Moreover, the nanocomposite PZT-Pt films in the capacitor configuration of Pt/LaNiO3/PZT-Pt/LaNiO3/Pt also exhibited highly reliable polarization retention and fatigue resistance.

A gas-phase synthesis route based on spray pyrolysis with a residence/heating time of less than 0.1 s was designed to directly prepare Eu-doped Y2O3 phosphor nanoparticles. The average size of the phosphor particles decreased from the submicron size to around 10 nm when the concentration of the starting solution was increased. By increasing the operating temperature, from 1500 to 1700 °C, the submicron-particles were converted into a nano-particle phosphor, and their photoluminescence intensities at 611 nm (254-nm excitation) were greatly improved. This synthesis procedure has considerable potential for preparing a variety of doped luminescent nanoparticles without the need for post-treatment processing.