The measured room temperature magnetic susceptibility of a bulk sample of buckytubes (buckybundle) is −10.75 × 10−6 emu/g for the magnetic field parallel to the buckybundle axis, which is approximately 1.1 times the perpendicular value and 30 times larger than that of C60. The experimental results are discussed in terms of a graphite-like electronic structure model.

Diamond films grown on {100}, {111} boron-terminated, and nitrogen-terminated facets of cubic boron nitride (c-BN) single crystals were characterized by Raman spectroscopy, scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The evolution of morphology and microstructure of the diamond films at different stages during the growth process were followed by SEM investigation. The results indicate that diamond growth proceeds by nucleation of oriented three-dimensional islands followed by their coalescence. Cross-sectional TEM specimens were prepared from thick (over 10 μm) continuous diamond films grown on {111} boron-terminated surfaces. Selected-area diffraction and high resolution TEM images show that the diamond film has a parallel orientation relationship with respect to the substrate. Characteristic defects, common to diamond films obtained by chemical vapor deposition on other substrates, are also discussed.

Cathodoluminescence (CL) spectroscopy in a scanning electron microscope was used to identify and to map the spatial distribution of luminescent defects in a synthetic diamond single crystal. Several defect CL bands were observed in the 1.5-3.5 eV region: (i) a band with a zero-phonon line at 2.156 eV, attributed to a center containing nitrogen and atomic vacancies; (ii) a broadband centered at ∼2.2 eV, tentatively attributed to a boron-containing center; (iii) a doublet line at 2.33 eV, attributed to a nitrogen-containing center; (iv) a zero-phonon line at 2.555 eV, attributed to a nickel-containing center; (v) a broadband centered at ∼2.85 eV, attributed to a dislocation-related center; and (vi) a zero-phonon line at 3.188 eV, attributed to a center containing nitrogen and a carbon interstitial. Lines due to free and acceptor-bound excitons were observed in the 5.0-5.4 eV region. The spatial variation of the CL was examined in the vicinity of regions of relatively high dislocation density (∼106 dislocations cm−2), which had been found in a previous x-ray diffraction imaging experiment. A quantitative analysis was made of the spatial variation of the band intensities. Upon moving from a relatively defect-free region to the center of a high dislocation density region, the intensities of defect bands (i) and (v) increased by very large factors (these bands were observed only within the high dislocation density regions); the intensity of defect band (vi) increased by a factor of ∼2; the acceptor-bound exciton intensity increased by a factor of 1.3; the intensities of defect bands (ii)-(iv) decreased by a factor of ∼2; and the free exciton intensity decreased by a factor of ∼7.5.

Ni(II)- and Co(II)-bearing ferrites with different levels of metal substitution have been studied for CO2 decomposition. Ni2+ and Co2+ have been substituted for Fe2+ or Fe3+ in magnetite with the spinel type of crystal structure up to 14% and 26% for the mole ratio of Ni2+ and Co2+ to the total Fe contents, respectively. The metal substitution was corroborated by Mössbauer spectroscopy and XRD studies. They were activated in a flow of H2 gas to form oxygen-deficient ferrites with the spinel structure retained. The oxygen-deficient M(II)-bearing ferrites have been found to show high reactivity toward CO2 decomposition to carbon at 300 °C. The reactivity increased with the level of metal substitution and activation. The oxygens of CO2 were incorporated into the spinel structure and carbon was deposited on the surface of the ferrites. The deposited carbon was visible on dissolution of the ferrites used. The rate of decomposition on H2-activated Ni(II)-bearing ferrite with the mole ratio of 14% was 30 times as high as that of H2-activated magnetite.

Ultrasonic propagation of longitudinal waves (CL mode) has been investigated as a function of temperature in a single crystal of a TaH0.51 hydride. Stepwise changes of the elastic constant CL and of the attenuation A have been observed in the vicinity of the β ↔ ∊ and ∊ ↔ α phase transitions. These changes occur over narrow temperature ranges corresponding to regions of coexistence of two phases. A relatively small temperature dependent softening is displayed by CL on approaching Tβ→∊ from the low temperature side. At the transition temperatures no divergency has been observed in the attenuation, which appears to originate from domain boundary motions, rather than from the transitions themselves. A determination of the H diffusion coefficient by a permeation method at high temperature supports a view that adiabatic tunneling is an effective mechanism even at temperatures as high as 1173 K.

Microwave plasma-enhanced chemical vapor deposition of diamond films on silicon carbide and tungsten carbide (with 6% cobalt) surfaces using fluorocarbon gases has been demonstrated. No diamond powder pretreatment is necessary to grow these films with a (100) faceted surface morphology. The diamond films are characterized by scanning electron microscopy and Raman spectroscopy. The proposed nucleation and growth mechanism involves etching of the noncarbon component of the carbide by atomic fluorine to expose surface carbon atoms and diamond nucleation and growth on these exposed carbon atoms. Hydrogen is necessary in the growth process to limit the rapid etching of the carbide substrates by corrosive fluorine atoms.

Kinetics and mechanism of sintering in a model borosilicate glass (BSG) + alumina composite system have been investigated isothermally at 600 to 1000 °C. A faster and greater densification is observed with higher sintering temperature, greater BSG content, and larger alumina particle size. Using measurable densification kinetics, it is found that the activation energy of densification (Q) increases continuously with increasing BSG content, from predominant <110 kJ/mol for BSG < 40 vol.% to 245 kJ/mol for BSG ≥ 90 vol.%. The rate-limiting step during densification is identified to be diffusion of alkali ions in BSG when BSG < 40 vol.% (Q = 110–170 kJ/mol), diffusion of both alkali and aluminum ions when BSG = 40–60 vol.% (Q = 110–170 kJ/mol), diffusion of aluminum ion in BSG when BSG = 60–80 vol.% (Q = 170 kJ/mol), and viscous flow of BSG when BSG ≥ 90 vol.% (Q = 245 kJ/mol). These observations are attributed to a chemical reaction taking place at the interface of alumina/BSG, resulting in a reaction layer adjacent to alumina. Since the composition of the reaction layer is known to be rich in aluminum and alkali ions and poor in silicon, the alkali ions content in BSG is continuously decreased during sintering. Accordingly, when the BSG content in the mixture is low, the resultant loss of alkali ions from BSG causes a rise in viscosity of BSG, thus slowing down the densification kinetics and changing the densification mechanism. As the amount of BSG is increased to ≥90 vol.% at the expense of alumina, the reaction as described above becomes less dominant and the sintering proceeds by viscous flow of glass.

A new process for the reactive ion etching (RIE) of both PbZr1−x TixO3 (PZT) thin films and RuO2 electrodes is presented, employing etching gases with low ozone depletion potential (ODP) and global warming potential (GWP). The etching process has been investigated as a function of etching time, discharge power density, chamber pressure, and additive gas. Etch rates were in the range of 250–650 Å/min and 100–400 Å/min for PZT and RuO2, respectively. A large etch selectivity between PZT and RuO2 was optimized. Etched surfaces exhibited smooth morphologies. Furthermore, the ferroelectric properties of PZT were not altered significantly by the etching process. A surface residue containing Cl and F was found after etching, but this organic substance was totally removed by an after-etch bake. In addition, the etched profile of the PZT films was studied through SEM.

A simple model for the size-dependent amplitude of the atomic thermal vibrations of a nanocrystal is presented which leads to the development of a model for the size dependent melting temperature in nanocrystals on the basis of Lindemann's criterion. The two models are in terms of a directly measurable parameter for the corresponding bulk crystal, i.e., the ratio between the amplitude of thermal vibrations for surface atoms and that for interior ones. It is shown that the present model for the melting temperature offers not only a qualitative but even an excellent quantitative agreement with the experimentally observed size-dependent superheating, as well as melting point suppression in both the supported and embedded metallic and semiconductor nanocrystals.

High quality Nd-doped single-mode fibers have been prepared by using a sol-gel process. The longest fluorescence lifetime measured was 520 μs in an Al: SiO2 glass fiber containing 0.47 wt.% neodymium oxide. An efficient neodymium fiber laser with a slope above threshold of 42% was successfully demonstrated with the sol-gel prepared Nd-doped single-mode fibers as a fiber laser oscillator.

Three coating techniques (metal-organic chemical vapor deposition, magnetron sputtering, and plasma-enhanced chemical vapor deposition) were employed to deposit different coating materials (alumina, a superalloy, and silicon nitride) on graphite-fiber-reinforced polyimide composites to protect against oxidation at elevated temperatures. Adhesion and integrity of the coatings were evaluated by isothermal aging (371 °C for 500 h) and thermal cycling (25 to 232 °C for 1000 cycles and −18 to 232 °C for 300 cycles). Best results were achieved with a plasma-deposited, amorphous silicon nitride (a-SiN: H) coating, which withstood stresses from 0.18 to −1.6 GPa. The major factors affecting the suitability of a-SiN: H as an oxidation protective coating are the surface finish of the polymer composite and the presence of a sizable hydrogen content in the coating.

An interparticle glass matrix in ruthenium dioxide-based thick film resistors has been studied intensively by means of analytical and high resolution transmission electron microscopy. The ruthenium dioxide phase interacts with lead-borosilicate glass at high temperature by dissolving ruthenium ions and incorporating a small number of lead and aluminum ions on the surface. Ruthenium ions diffuse through the glass network at least over a distance of 1 μm during firing, but are accommodated in the glass structure by an amount only less than 7 at. % at room temperature. High resolution electron microscopy reveals numerous ruthenium-pyrochlore crystallites in high-lead glasses, but hardly any Ru-based clusters/crystallites in low-lead glasses, where lead-rich glass clusters due to glass immiscibility and reduced lead metal clusters are more commonly observed instead of ruthenium clusters. Lead oxide is prone to reduction both in high- and low-lead glasses upon irradiating with a high-energy incident electron beam. Comparison with gold-based resistor and estimation of average dispersion length of ruthenium clusters, 2 to 4 nm, prefer the model of electron hopping via ruthenium clusters/crystallites as a dominant conduction mechanism in thick film resistors.

Diffusion barriers of silica were deposited on soda-lime glass using a sol-gel technique. The migration of sodium from the glass through these layers and into a spray-pyrolyzed layer of fluorine-doped tin oxide was studied by SIMS depth profiling. The silica layer reduced sodium in the tin oxide overlayer by two orders of magnitude.

Oxyreduction studies of mixed Ce/Pr oxides have been carried out. Temperature-programmed desorption (TPD), temperature-programmed reduction (TPR), and temperature-programmed oxidation (TPO) were used to study the uptake and release of the oxygen. Large amounts of oxygen, exceeding those in ceria, are accessible in the mixed metal oxides at moderate temperatures. The addition of small amounts of noble metals to the mixed oxides shifts the accessibility of the “stored” oxygen to still lower temperatures with the effect of Pd being more pronounced than that of Pt. In a sample containing 45 mol % ceria and 55 mol % praseodymia, a small addition of Pd (0.24 mol %) was found to lower the reduction temperature by more than 100 °C. The addition of Pt had a lesser effect. Similarly, in pure praseodymia (Pr6O11) Pd influences the reduction much more strongly than Pt. In the mixed samples, whether doped with a noble metal or not, the whole oxyreduction effect can be accounted for by the change in oxidation state of the praseodymium ions solely. This notwithstanding, the reduction of the mixed oxides, without noble metals or doped by Pt, is more facile than that of praseodymia. Only the incorporation of Pd makes the reduction of praseodymia proceed at a temperature below that registered for a mixed ceriapraseodymia sample.

We report scanning tunneling microscope images of gold-coated fracture surfaces of soda lime glass and fused silica in the mirror region. The scans show a variety of nanometer scale features that are attributed to fracture phenomena at this scale. We find considerable similarity to the structures observed in regions of extensive crack branching (e.g., “mist”). The density of these features increases as one progresses away from the crack origin toward the mirror-mist boundary. Comparisons are made between soda lime glass and fused silica, revealing differences in the local deformation behavior of these two materials. Self-similarity of the observed structures is probed by measurements of the fractal dimension, Df, of the surfaces created in soda lime glass near the mirror-mist boundary, where we observe 2.17 > Df > 2.40.

It has been found that electric field induced fibrolysis of suspended dielectric powder in a variety of uncured thermoset polymeric materials is a potential fabrication means to assemble ceramic-polymer composites. The resulting composite material consists of a quasi 1–3 connectivity pattern due to the formation of fibrils by the ceramic powder. For a given thermoset polymer, the degree to which these fibrils form is strongly dependent on both the magnitude and frequency of the applied field. Fibril formation is maximized at certain ac frequencies independent of the volume fraction of filler utilized. Outside these frequency ranges, electroviscous behavior and the associated fibrolysis are drastically diminished or even nonexistent. The critical frequency values and their relation to the ideal assembly conditions for this class of composite materials are the focus of this paper.

Fe-Cr/Al2O3 metal-ceramic composites prepared by hydrogen reduction at different temperatures and for different periods have been investigated by a combined use of Mössbauer spectroscopy, x-ray diffraction, transmission electron microscopy, and energy-dispersive x-ray spectroscopy in order to obtain information on the nature of the metallic species formed. Total reduction of Fe3+ does not occur by increasing the reduction time at 1320 K from 1 to 30 h, and the amount of superparamagnetic metallic species is essentially constant (about 10%). Temperatures higher than 1470 K are needed to achieve nearly total reduction of substitutional Fe3+. Interestingly, iron favors the reduction of chromium. The composition of the Fe-Cr particles is strongly dependent on their size, the Cr content being higher in particles smaller than 10 nm.

Reflection electron energy loss spectroscopy (REELS) and optical reflectivity measurements have been used to characterize in the valence energy region the dielectric behavior of 7-amino-2,4 dimethyl-1,8 naphthyridine and of the charge transfer complex formed by this compound and the 7,7',8,8'-tetracyanoquinodimethane (TCNQ). The effects of the charge transfer interaction on the core energy levels have been investigated by comparing the line shape of the carbon and nitrogen Is core photoelectron peaks of the electron-donor and electron-acceptor molecules and of the charge transfer complex formed by them.

The impact code EPIC was employed to study the relationship between the applied force and the penetration depth in a micrometer-scale indentation experiment with oxygen free high conductivity (OFHC) copper. EPIC is an elastic-plastic finite element code that uses a Lagrangian formulation and triangular mesh, which can accommodate large deformation without the need to remesh during the computation process. By fitting the force-penetration curves for a triangular indenter with second degree polynomials, it was demonstrated that the fit changed with two material constants in the constitutive equation. A systematic procedure for determining the material constants is described that is based on matching either the slope or the curvature of the force penetration depth curves from numerical simulation and experiments. It is concluded that material constants can be determined from indentation data obtained using pyramidal or spherical indenters as well as a flat-ended indenter.

β-SiC whiskers were synthesized by the vapor-liquid-solid (VLS) process using Fe catalyst. Whiskers show smooth surfaces and no ramifications. They have uniform diameter (0.5-1 μm) and lengths between 50 and 300 μm. A catalyst droplet was observed on the tip of almost all the whiskers. The transport of iron from the substrate surface to the SiO generators, where growth took place, occurs fundamentally via vapor phase. Fe was deposited over surfaces containing C, and whisker growth was produced where there were Fe droplets of appropriate size and SiO available in great quantity. The need for reaching a threshold size (2–3 μm) of the catalyst droplet before whisker growth is proposed as a possible explanation for the formation of whiskers with uniform size in zones with a high partial pressure of SiO.