We demonstrated rapid prototyping of templates for replica molding using a conventional laser printer. A polymer, polydimethylsiloxane, was cast directly on the transparency templates to make the replicas. The templates and replicas were characterized by scanning electron microscopy, profilometry, and optical microscopy. Four patterns, including an Electronic Industries Association resolution test pattern, were printed on transparencies at 600 dots per inch on a HP LaserJet 4M printer (Hewlett-Packard, Palo Alto, CA). Optimal precision and clarity occurred between intensity settings of 50–100. Mean pattern height/depth ranged from 8–13 μm, and width was as small as a few tenths of a millimeter. Mean surface roughness of the template patterns ranged from 1 to 4 μm on the top surface and from 5 to 10 nm on the bare transparency surface. This method provides access to microfabricated patterns for the broader research community without the need for sophisticated micromachining facilities.

Smooth polycrystalline diamond films were deposited onto silicon substrates using a newly developed time-modulated chemical vapor deposition (TMCVD) process. The distinctive feature of the TMCVD process involves pulsing the hydrocarbon gas, methane, at different flow rates for varying durations into the vacuum reactor during the chemical vapor deposition (CVD) process. Generally, CVD diamond films display nonuniformity in the crystal sizes and surface roughness along the film growth profile. The TMCVD method was specifically developed to (i) deposit smooth films, (ii) control film microstructure and morphology, and (iii) improve film reliability. We show that the TMCVD process produces diamond films with improved surface smoothness as compared to films of similar thickness produced by conventional CVD method under similar conditions. Surprisingly perhaps, the TMCVD method gave growth rates much higher than the conventional CVD method without reducing the film quality as revealed by the SEM micrographs and micro-Raman spectra.

The direct observation of a type of microstructure in the organic matrix layers of nacre was obtained with a transmission electron microscope. The microstructure, which is referred to as mineral bridge in the biomineralization, is nanoscale and randomly distributed in the layers. Statistical analysis gives the distribution laws and characteristics of mineral bridges in the organic matrix layers. The existence of mineral bridges in nacre was confirmed, and it was shown that the microarchitecture of nacre should be described as a “brick–bridge–mortar” arrangement rather than traditional “brick and mortar” one.

HfO2–SiO2 and La2O3–SiO2 amorphous alloys were prepared, and their crystallization behavior was studied. The results suggest that higher permittivities can be achieved in the La-containing system without devitrification. The crystallization mechanisms between systems are distinctly different, yet observations are consistent with bulk material. Hf-containing materials tend toward phase separation, while La-containing materials tend toward silicate formation. For Hf-containing films, negligible thickness or time dependence was observed. In La-containing films, rapid thermal anneals could improve crystallization resistance, and thickness effects related to interface reactions were observed. These behaviors are discussed in the context of phase diagrams and metastable immiscibility.

This paper investigates the possibility of reducing the deposition temperature of polycrystalline silicon germanium to a level compatible with complementary metal-oxide semiconductor (CMOS) post processing. To achieve this goal, the exact wafer temperature during deposition was experimentally determined and it was found to be 30 °C lower than the reactor setting temperature. The deposition temperature was reduced from 625 to 500 °C. The impact of varying the deposition pressure from 10 to 760 torr and the germanium content from 15% to 100% was investigated. X-ray diffraction spectroscopy and transmission electron microscopy showed that the SixGe1−x films deposited at an actual wafer temperature of 520 °C are polycrystalline for germanium contents as low as 15%. Also, it was shown that the deposition conditions can be adjusted to yield a low tensile stress at an actual wafer temperature of 520 °C, which is suitable for integrating surface micromachined micro-electromechanical systems on top of standard CMOS wafers with Al interconnects.

The single crystals of a binary organic 1:1 molecular complex were grown from different solvents. The single crystal x-ray diffraction study revealed that the binary material has crystallized with a noncentrosymmetric space group (P21) entirely different from that of the parent components. Second harmonic generation measurement on polycrystalline material shows green light emission with the molecular complex. The differential scanning calorimeter and the thermogravimetric analysis show eminent higher melting point and decomposition temperature, respectively for the binary molecular complex compared to that of urea and m-nitrobenzoic acid. The optical spectrum of newly grown crystal shows the cutoff wavelength (398 nm) near the UV region, and the micro hardness measurement confirmed the greater hardness of the binary crystal.

Dense 3-mol%-yttria-stabilized tetragonal zirconia polycrystals (3Y-TZP/Ni) homogeneous composites were prepared by a wet-processing route with metal concentration ranging from 0 to 40 vol%. Cyclic fatigue stress/life, tensile and bending strength, and fracture toughness were investigated in 3Y-TZP monolithic samples and 3Y-TZP/Ni composites. It was found that the addition of Ni particles to the 3Y-TZP matrix produced an embrittlement effect in the composites, decreasing the mechanical properties. This fact was attributed to the weak bonding between the Ni and 3Y-TZP particles in samples sintered in a reductive atmosphere. Additionally, the presence of Ni particles decreases the cyclic tensile fatigue of the composites probably by an environmentally assisted slow crack growth.

We have examined galena powders with the aim of providing information about the preparation mode of such powders from ancient Egyptian burial objects. Two extreme conditions of milling have been used to prepare galena powders in the laboratory, and the resulting products have been examined using scanning electron microscopy and transmission electron microscopy (TEM). The microstructure of hand-crushed coarse particles consists mainly of dislocation tangles. Annealing at 300 °C promotes a substantial recovery of the dislocation structure with the formation of subboundaries. Energetic ball milling produces a large variety of particle sizes, from 10 nm to several micrometers, with grains containing very high dislocation densities. Although PbS is a soft plastic compound, its fragmentation occurs down to very small sizes along various fracture regimes like in many brittle materials. Comparisons are made between TEM observations and the data obtained from x-ray diffraction peak profile analysis.

The evolution of interfacial microstructure of eutectic SnAgCu and SnPb solders on Al/Ni(V)/Cu thin films was investigated after various heat treatments. In the eutectic SnPb system, the Ni(V) layer was well protected after 20 reflow cycles at 220 °C. In the SnAgCu solder system, after 5 reflow cycles at 260 °C, the (Cu,Ni)6Sn5 ternary phase formed and Sn was detected in the Ni(V) layer. After 20 reflow cycles, the Ni(V) layer disappeared and spalling of the (Cu,Ni)6Sn5 was observed, which explains the transition to brittle failure mode after ball shear testing. The different interfacial reactions that occurred in the molten SnAgCu and SnPb systems were explained in terms of different solubilities of Cu in the two systems. The dissolution and formation of the (Cu,Ni)6Sn5phase were discussed on the basis of a Sn–Ni–Cu phase diagram. In the solid-state aging study of the SnAgCu samples annealed at 150 °C for up to 1000 h, the Ni(V) layer was intact and the intermetallic compound formed was Cu6Sn5 and not (Cu,Ni)6Sn5, which is the same as was observed for the eutectic SnPb system.

Nanostructured montmorillonite/poly(diallyldimethylammonium chloride) multilayer thin films were fabricated up to 100 layers thick by stepwise alternating polyelectrolyte and clay deposition from solution. The structure and morphology of the films were characterized by x-ray diffraction, ellipsometry, atomic force microscopy, and quartz crystal microbalance ex situ and in situ measurements. The mechanical properties were tested by nanoindentation. The hardness of the multilayer thin film was 0.46 GPa. The thin film's modulus was correlated to its ordering and anisotropic structure. Both hardness and modulus of this composite film were higher than those of several other types of polymer thin films.

In this article, we report formation of separation-by-implantation-of-oxygen (SIMOX) silicon-on-insulator (SOI) materials with doses ranging from (2.5 to 13.5) × 1017 cm−2 at acceleration energies of 70–160 keV and subsequent annealing at temperatures over 1300 °C in oxygen + argon atmosphere for 5 h. The microstructure evolution of SIMOX wafers was characterized by Rutherford backscattering spectroscopy, cross-sectional transmission electron microscopy, high-resolution transmission electron microscopy, Secco, and Cu-plating. This study revealed a series of good matches of dose-energy combination at acceleration energies of 70–160 keV with doses of (2.5–5.5) × 1017 cm−2, in which SIMOX wafers had good crystallinity of the top silicon, sharp Si/SiO2 interfaces, high-integrity buried oxide layers with low pinhole density, and low detectable silicon islands. Furthermore, the higher the oxygen dose, the higher the implanted energy required for the formation of a buried oxide free from Si islands. The mechanism of the optimum dose-energy match is discussed.

Highly textured zinc oxide films were produced on basal plane sapphire substrates by chemical solution deposition. Films with oriented growth were achieved by spin coating a 0.75 M precursor solution of zinc acetate dihydrate and ethanolamine in 2-methoxyethanol, heated at 300 °C/10 min, then at 500 °C/5 h, and finally at 850 °C/12 h. Films were characterized with x-ray diffraction (XRD) and scanning and transmission electron microscopy. The films exhibited only the (0002) ZnO line in XRD diagrams, proving a very well-developed out-of-plane texture. At temperatures above 700 °C the ZnAl2O4 spinel was observed, which formed as a reaction layer between sapphire and ZnO. Few specimens produced both in-plane and out-of-plane oriented growth of ZnO on basal plane sapphire. It was hypothesized that the substrate miscut, uncontrolled for the current experiments, could be the cause of the infrequent growth of epitaxial films.

Plastic deformation of Pd–40Ni–20P bulk metallic glass (BMG) was investigated by instrumented nanoindentation experiments over a broad range of indentation strain rates. At low rates, the load–displacement curves during indentation exhibited numerous serrations or pop-ins, but these serrations became less prominent as the indentation rate was increased. Using the tip velocity during pop-in as a gauge of serration activity, we found that serrated flow is only significant at indentation strain rates below about 1–10/s. This result suggests a transition in plastic flow behavior at high strain rates, in agreement with prior studies of BMGs under different modes of loading.

A planetary ball-mill device that enables one to perform solid-gas reactions at constant pressure was developed. Titanium powders were ball milled under nitrogen at a spinning rate of 960 rpm. The influence of the nitrogen pressure on the mechanochemical reactivity of titanium was analyzed at 1.5 and 11 bars. A spontaneous combustion took place during the grinding process, leading to a high yield of TiN for short milling times. The conversion of titanium into titanium nitride was facilitated by increasing the nitrogen pressure. At 11 bars, full conversion was reached for grinding times shorter than 5 h. Titanium nitride obtained in this way exhibited a high sintering activity.

Some tungsten-bronze compounds in the BaO–Nd2O3–TiO2–Nb2O5 system were prepared and characterized. Ba4Nd2Ti4Nb6O30 and Ba5NdTi3Nb7O30 had the filled tetragonal tungsten-bronze structure, and Ba3Nd3Ti5Nb5O30 consisted of the tetragonal tungsten-bronze major phase and a minor amount of secondary phase BaNd2Ti3O10. These compounds had significant relaxor behaviors, and the Curie temperatures (at 1 MHz) were 0 and 55 °C for Ba3Nd3Ti5Nb5O30 and Ba5NdTi3Nb7O30 ceramics, respectively. A high dielectric constant (213) combined with low dielectric loss (0.004 at 1 MHz) was obtained in Ba3Nd3Ti5Nb5O30 ceramics. In addition, the solid-solution range of BapNd6−pTi8−pNb2+pO30 was 3 < p ≤ 6.

Phase formation and thermal stability for an Al–Mn–Be alloy have been investigated by melt-spinning and conventional casting. Significant differences in the phase formation and the thermal stability of the microstructure were found as a result of the different cooling rates. In the melt-spun ribbons, a large volume fraction of a metastable icosahedral phase was found to coexist with an Al solid solution. In the bulk cast ingots, the primary phase formed in the two-phase microstructure was a hexagonal approximant phase of quasicrystals. This phase that solidified in the form of faceted particles embedded in the Al solid matrix proved to be thermodynamically stable during annealing at 540 °C for 100 h. The effect of Be addition on the formation of the stable approximant phase is discussed in terms of the Hume–Rothery mechanism.

Biaxially textured <100>-oriented SrTiO3 films were solution deposited on <100> LaAlO3 single crystals and <100>-oriented polycrystalline Ni tapes. Solution variables including varying titanium alkoxide chain length, inclusion of chelating agents, and inclusion of donor dopant, were investigated for their effect on film orientation, morphology, and oxygen diffusivity. The best <100> SrTiO3 orientation on high lattice mismatch (11%) Ni substrates was achieved through use of a discontinuous nucleation seed layer, which provided nucleation sites for subsequent continuous SrTiO3 films. Increased titanium alkoxide chain lengths appeared to suppress titanium hydrolysis reactions and improve film orientation. 13C nuclear magnetic resonance showed that significant quantities of water were generated due to esterification reactions, which appeared to cause hydrolysis and subsequent orientation degradation in the absence of chelating agents such as acetylacetone.

Increased ionic conductivity at nanoscale planar interfaces of the CaF2|BaF2 system was successfully modeled using molecular dynamics simulations. A criterion was established to construct simulation cells containing any arbitrarily lattice-mismatched interfaces while permitting periodic boundary condition. The relative (to the bulk) ionic conductivity increase at the 111 (CaF2)|111 (BaF2) interface was qualitatively reproduced. Higher conductivity, by a factor of 7.6, was predicted for the 001 (CaF2)|001 (BaF2) interface. A crystalline nanocomposite of the CaF2|BaF2 system, in which the [001] morphology is encouraged and crystallite dimensions are approximately 4 nm, was proposed to give ionic conductivity approaching that predicted for the 001 (CaF2)|001 (BaF2) interface.

A novel method was developed for low-temperature preparation of thin films. Pulsed laser ablation was combined with electron cyclotron resonance microwave discharge, constituting a novel hybrid film preparation method called electron cyclotron resonance plasma–assisted reactive pulsed laser deposition. We demonstrated the feasibility of the method by preparing compound films of silicon nitride, silicon dioxide, and aluminum nitride from elemental starting materials. The mechanisms responsible for efficient compound formation and film growth are discussed, together with characterization of the prepared films, analysis of the plasma composition, and comparison of the films prepared with and without assistance of the plasma. The unique features of the method make it suitable for one-step preparation of compound thin films at low temperatures.

Antimony oxide nanorods were synthesized by the microemulsion method. The nanorods had diameter in the range of 507–175 nm and a length of up to several micrometers. The microstructure of the nanorods was examined by analytical transmission electron microscopy and high-resolution transmission electron microscopy (HRTEM). Large-angle tilt diffraction experiments on the normal nanorods (about 90 nm in diameter) showed that they have an orthorhombic structure. Combining the results of internal standards using the silicon single crystal, it could be concluded that the synthesized nanorod is Sb2O4. The common growth direction of the nanorods was along the long axis. HRTEM images showed it had a periodic layer structure, and some defects and a layer of amorphous on the nanorods surface were found. The formation mechanism of Sb2O4 nanorods is briefly discussed.