Carbon films with up to 32 at. % of nitrogen have been prepared with ion beam assisted magnetron, using a N2+/N+ beam at energies between 50 and 300 eV. The composition and density of the films vary strongly with the deposition parameters. EELS, SXS, XPS, and IR studies show that these a-C: N films are mostly graphitic and have up to 20% sp3 bonding. Nitrogen is mostly combined with carbon in nitrile (C ≡ N) and imine (C=N) groups. It is shown by RBS and NDP that density goes through a maximum as the average damage energy per incoming ion increases. Positron annihilation spectroscopy shows that the void concentration in the films goes through a minimum with average damage energy. These results are consistent with a densification induced by the collisions at low average damage energy values and induced graphitization at higher damage energy values. These results are similar to what is observed for Ar ion assisted deposition of a-C films. The mechanical properties of these films have been studied with a nanoindenter, and it was found that the hardness and Young's modulus go through a maximum as the average damage energy is increased. The maximum of mechanical properties corresponds to the minimum in the void concentration in the film. Tribological studies of the a-C: N show that the friction coefficient obtained against diamond under dynamic loading decreases strongly as the nitrogen composition increases, this effect being more pronounced at low loads.

Ferroelectric Pb[(Mg1/3Nb2/3)0.7Ti0.3]O3 (abbreviated PMNT) thin films were prepared on silicon substrates by rf magnetron sputtering deposition with PbO-enriched PMNT targets. The effects of electrode composition and thin film growth conditions were investigated with grazing-incidence x-ray diffraction, secondary ion mass spectrometry, and scanning electron microscopy. The dielectric property of perovskite films was also measured. The usage of a Pt/Ti electrode was observed to enhance the formation of perovskite PMNT films; in addition, the TiO2 rutile phase was formed at the interface between the PMNT film and Pt electrode due to the oxidation of out-diffused Ti atoms from the inner Ti electrode. It was then noticed that if a target containing a larger excess of PbO was used, a higher consumption of TiO2 occurred and more perovskite phase would be formed in the deposited films. Consequently, perovskite PMNT films having a uniform microstructure and satisfactory dielectric property close to the bulk value were obtained by rf magnetron sputtering deposition on the Pt/Ti/SiO2/Si substrate at 640 °C under appropriate working conditions.

Cd-arachidat in the form of Langmuir-Blodgett films and thick photoresist layers of AZ5412H have been exposed to 15N-ion beams. The physico-chemical state of these targets as a function of the 15N fluence has been monitored by the 15N nuclear reaction with the respective H component. In this way, radiolytic changes in H distribution and bonding have been measured. In particular, diffusion and desorption processes have quantitatively been followed up to fluences of about 1 × 1016 N/cm2 at temperatures as low as 40 K. The correlated changes in H bonding, obtained by analyzing the concomitant Doppler widths as a function of the 15N fluence, consist of both decomposition and restoration of C-H and H-H molecular groups.

The early stages of microwave-plasma assisted CVD of diamond on fused silica and silicon substrates were investigated. Nucleation densities on fused silica were somewhat lower than on silicon; however, the diamond growth rates on fused silica were faster. These results suggest that the substrate alters the plasma chemistry near the substrate. Transmission electron microscopy showed a relatively smooth interface between the diamond grains and the SiO2 surface. At low nucleation densities, the growth kinetics on both substrates were linear (i.e., the average feature size was proportional to the deposition time), which indicates that the growth kinetics were initially controlled by reaction(s) at the growing diamond surfaces. The transition to nonlinear growth kinetics observed at higher nucleation densities was probably caused by mass-transport limits.

Swirls and oxidation stacking faults (OSF) ring-bands in the near surface region of Si crystals have been detected and characterized by a 180°backscattering Rayleigh-Brillouin spectrometer using an argon-ion laser as its light source. In FZ Si wafers with swirls, the central region exhibits high scattered light with random undulation, the peripheral region with swirls shows a periodic undulation of scattered light intensity, while the region in-between is a nearly uniform zone of low scattered light intensity. In contrast to this, the CZ Si wafers with OSF ring-bands display a low uniformly scattered light background with a high undulated scattered light zone corresponding to the OSF ring-band. The scattered light intensity and its structure in the OSF ring-band vary with the heat-treatment conditions. The features of scattered light detected by the scattering spectrometer are discussed.

A new process for ion implantation into silicon wafers was proposed. This process has an additional implantation step to form an amorphous phase. At first self-ions are implanted into a cooled wafer (< −30 °C) to form the amorphous phase, and subsequently dopant atoms are implanted to form a doped layer within the amorphous layer. After annealing above 650 °C, the silicon wafer is completely recrystallized, and no defects with sizes detectable by TEM are present near the doped layer. There is indeed a defect layer in the wafer; however, it lies along the amorphous/crystal interface that is behind the doped layer. The concentration profile of the dopant atoms is not changed during epitaxial recrystallization, and further dopant atom diffusion during annealing is limited to about 0.05 μm, because defect-enhanced diffusion does not occur. The double implantation method is considered to be effective for doped layer formation in the VLSI fabrication process.

A low cost, highly versatile electron backscattering diffraction system has been developed for an ElectroScan E3 Environmental Scanning Electron Microscope (ESEM). A P20 phosphor coated screen is placed in the microscope environment to image electron backscattering diffraction patterns (EBSP's). A CCD TV camera is used to view the patterns through a leaded glass port in the microscope specimen chamber. This system has a spatial resolution approaching 5 μm and yields analyzable patterns at pressures of up to 6 Torr. With minor modifications this system may be adapted to fit any scanning electron microscope. Comparison of analyses of the grain boundary misorientation of a Ni-16Cr-9Fe alloy with this system and by selected area channeling patterns (SACP's), performed in a standard SEM, yielded excellent agreement between the two techniques. Owing to the capability to perform on-line analysis of EBSP's, the EBSP technique required only half the time as the SACP technique. The capabilities of the system are illustrated in a study of the grain boundary character distribution of Ni-16Cr-9Fe following thermomechanical treatment.

There is currently considerable interest in producing high temperature capability graphitic materials by first weaving graphite fiber tows (yarns) into a “preform” structure, followed by densification via cracking of precursor compounds such as dimethyldichlorosilane within the pores (macro and micro) at high temperature. The model described in this paper addresses this densification process, treating diffusion of gaseous species both within the macropores (spaces between the tows) and the micropores (spaces between individual fibers in the tows) and finite kinetics associated with the cracking of the precursor gas (treated parametrically). The resulting model is used to examine the effects of temperature distributions through cylindrical preforms on ultimate densification distribution. As might be expected (and as observed experimentally), uniform temperature through the preform leads to premature full densification of the pore structure at the periphery of the cylinder (blocking further densification in the interior), leading to severe porosity in the interior regions. Effects of externally imposed nonuniform temperature profiles (possibly via microwave heating) in alleviating this problem are examined, and it is shown that proper profiling can lead to nearly complete uniform densification throughout the preform.

Electron diffraction intensities from cylindrical objects can be conveniently analyzed using Bessel functions. Analytic formulas and geometry of the diffraction patterns from cylindrical carbon nanotubes are presented in general forms in terms of structural parameters, such as the pitch angle and the radius of a tubule. As an example the Fraunhofer diffraction pattern from a graphitic tubule of structure [18,2] has been simulated to illustrate the characteristics of such diffraction patterns. The validity of the projection approximation is also discussed.

Densification kinetics and mechanism of a binary borosilicate glass composite, containing low-softening borosilicate (BSG) and high-softening high silica (HSG) glasses, have been studied. Apparent activation energy of densification varies from 200 to 400 kJ/mol, and decreases with increasing BSG content at a given densification factor. At a given BSG content, the activation energy of densification initially remains relatively unchanged with increasing densification factor (DF), but increases with densification when DF reaches a critical value (DF∗). Moreover, the value of DF∗ increases with increasing BSG content. From the activation energy estimates of densification, it is concluded that the predominant densification mechanism for BSG ≥ 30 vol. % with DF < DF∗ is viscous flow of low-softening BSG. For BSG ≥ 30 vol. % with DF < DF∗ and BSG ⋚ 20 vol. % with all DF investigated, the activation energies are within the range governed by viscous flow of both BSG and HSG, indicating that the densification is controlled by viscous flow of a new glass with a composition between BSG and HSG. The latter evidence stems from the microstructural observation that as sintering proceeds, the HSG particle undergoes an extensive dissolution process.

Films of PbO/MoS2, grown by pulsed laser deposition, exhibit a significant improvement in tribological performance compared to MoS2 films grown by the same process. The microstructure and crystallography of PbO/MoS2 composite films were investigated using transmission electron microscopy (TEM) to identify the features responsible for this tribological improvement. Self-supporting samples were prepared from pulsed laser deposited, PbO/MoS2 thin films grown on single crystal sodium chloride substrates. Films deposited at room temperature exhibited a two-phase microstructure with one of the phases being amorphous. X-ray microanalysis results showed that the crystalline phase had significantly higher concentration ratios of Mo/Pb, Mo/S, and Pb/S than did the amorphous phase. Films grown at 300 °C were polycrystalline, with a grain size of about 20 nm, and had a NaCl type structure which was isomorphous to PbS. The grains had rectangular shape, and exhibited preferred orientation with the sodium chloride substrate. The concentration of S for these films was approximately 80% of the S concentration for films grown at room temperature. Both the high temperature and room temperature films had S concentrations which were higher than expected from the MoS2 in the target; this was attributed to gettering of the S in the vacuum chamber by Pb. The electron diffraction results, together with previously published results, suggest that the crystal structure of the phases in these films is not responsible for the improvement in tribological properties. However, the microstructural components formed during film growth do determine the wear-induced chemical reaction pathways.

We recently performed a series of experiments on Nb-doped lead-zirconate-titanate ceramic to investigate the influence of constant shear stresses on the displacive, first-order rhombohedral/ferroelectric → orthorhombic/antiferroelectric polymorphic transformation. In a previous paper and report we demonstrated that increasing shear stresses lowers the mean stress and confining pressure at which the transformation occurs, but we did not identify a criterion by which the transformation could be predicted to take place under nonhydrostatic stress. In this paper we use the dielectric anomaly which accompanies the transformation as an indicator of onset of the transition, and correct for the effects of high-pressure-seal friction on measurement of the maximum compressive stress applied to the test specimens during deviatoric loading. We show that a convincing case can be made that the transformation occurs when the maximum compressive stress equals the hydrostatic pressure at which the transformation would otherwise occur.

Thermal stresses induced during cooling from temperatures used for coating deposition were calculated for various fiber-coating systems. Systems under study include several types of carbon, alumina, and zirconia fibers. Coatings considered were TiB2, Si3N4, and SiC. Typical calculated stresses were on the order of 0 to 2 GPa. The results were used to analyze the effects of variable physical parameters such as coating thickness and crystallographic orientation on the stress levels. Each fiber-coating system was then compared using a nominal coating thickness of 5 μm in order to rank the various fiber-coating combinations. Among the results obtained, it was shown that orientation of deposited coatings usually leads to higher tensile stresses.

“Heteroepitaxy of rare-earth hexa-aluminates on sapphire” [J. Mater. Res. 9, 410-419 (1994)]

In this three-part series the compressive behavior of (i) glassy polymers, (ii) high performance polymeric and carbon fibers, and (iii) polymeric matrix composites has been addressed. The glassy polymers exhibit plastic yielding in compression. The dependence of compressive yield strength on factors such as tensile modulus, glass transition temperature, density, and free volume has been examined. Failure theories for yielding in glassy polymers have been reviewed. Compression behavior of high performance fibers and that of the composites is discussed in Parts II and III, respectively.

Simultaneous measurements of thermal conductivity and diffusivity of ferroelectric polycrystalline samples of the KDP family type have been performed with the transient plane source (TPS) technique over the temperature range 88-300 K. The thermal conductivity behavior resembles that of the corresponding single crystals, but with values a factor of three lower. This decrease in thermal conductivity of the polycrystalline form is attributed to scattering mechanisms due to microstructural imperfections such as point defects, grain boundaries, etc. Values of porosity have been estimated using the dimensions of the unit cell deduced from the x-ray analysis and the apparent densities. The data indicate that the phase transition mechanisms (displacement type and order-disorder type) still dominate the conduction processes in spite of the presence of other scattering mechanisms due to the imperfection of the microstructure in the polycrystalline form of these materials.

CdTe microcrystallites were precipitated in 57.8CdO · 19.7SiO2 · 19.0B2O3 · 3.5Al2O3 glasses doped with 5.0 mol % CdTe. The microcrystallite size increased linearly with t1/3 (t: heat-treatment time), indicating diffusion-controlled growth mechanism, where the estimated activation energy for diffusion was 542 kJ/mol. The linear increase in the band gap energy with l/r2 (r: the crystallite radius) suggested the quantum size effect of the CdTe microcrystallites.

In this study, we have investigated the microwave dielectric behavior of a composite formed by embedding nickel-coated graphite fibers in an epoxy matrix. Permittivities of composites in the X-band frequency range as a function of fiber concentration, fiber length, and the degree of fiber aggregation were studied. Fiber aggregation was reduced significantly by the addition of silica particles to the composite mixture before epoxy curing. Predictions from the mean field theory fit the experimental data well at dilute fiber concentrations.

SQUID magnetometer characterization of Ca–Ni–K–O catalyst materials reveals complex magnetic behavior. The magnetic properties are generally determined by the antiferromagnetic material NiO, but samples with traces of elemental nickel show marked effects of ferromagnetism. Potassium doping enhances the formation of metallic nickel. Further deviations from bulk NiO properties can be attributed to NiO particle size effects (superparamagnetism) and to the presence of paramagnetic impurities, possibly Ni3+ ions.

A micro-impact tester has been designed and built by using a piezoelectric impact hammer as an impactor driver. During the course of an impact process, force interactions between the impactor and target surfaces were monitored continuously by a miniaturized piezoelectric loadcell embedded in the flying head assembly. A 3-sided pyramidal diamond indenter (Berkovich indenter) was used as an impactor. After having fully characterized such an impact system, the trajectory of the impactor can be calculated by using the corresponding prerecorded impact force interaction in a simulation program. The contact and returning velocities, kinetic energy loss of the impactor, and the impact penetration curve are the key pieces of information obtained from the simulation. Furthermore, the impact morphology can reveal failure mechanisms of materials by providing details such as indent shapes, coating fragment, chipping, crack type and size, and other information which are useful in assessing the fracture toughness of testing materials. The micro-impact testing was carried out in the contact velocity ranging from 0.3 to 2.0 m/s. Three types of materials such as metal, glass, and amorphous carbon were used in studying their distinct mechanical behavior under high rate indentations. The correlations among the impact conditions, energy losses, impact morphologies, and material responses are illustrated and discussed.