With the growing potential for use of Bi-2212 powders in high temperature superconducting applications, it is important to understand the processing characteristics of the material. To meet this need, the present work established the relationship between confining pressure and green density for powders of different particle sizes and morphologies. Mechanical properties, including elastic and plastic behavior, of the resulting green compacts were also measured as a function of relative density. Particle size and size distribution are shown to have a significant impact on the properties of interest. The implications of such findings are discussed with respect to the powder-in-tube process for making high temperature superconducting wire and tape.

Sr-doped Pr1.85Ce0.15CuO4+δ samples have been prepared with accurate control of the oxygen content. The stability of both T′ and T* phases is strongly dependent on Sr and oxygen content. An electron diffraction study indicates that, in some cases, anionic vacancies are ordered leading to a pseudo-tetragonal superlattice with unit cell parameters . Structural transitions and superconducting phases created by hole doping in such a system are also reported.

We have investigated the stability of the (Bi, Pb)2Sr2Ca2Cu3Ox phase for the stoichiometry (Bi: Pb: Sr:Ca: Cu = 1.72: 0.34: 1.83: 1.97: 3.13), subjecting it to temperatures between 700 and 850 °C under various oxygen partial pressures. A narrow region was found in which Bi, Pb(2223) was the only superconducting phase. This region follows closely the thermal decomposition line. X-ray pure Bi, Pb(2223) will partially decompose if treated outside of the stability region. For a given oxygen partial pressure, the Bi, Pb(2223) phase tends to coexist with the 2201 phase for temperatures above, and the 2212 phase for temperatures below this region. At even lower temperatures an additional lead-rich phase appears. Critical temperatures Tc vary little with treatment and range between 108.5 K and 110.8 K. If 10% silver is added to the starting powder, the phase coexistence regions shift. Silver does not seem to have a significant effect on the absolute values of the critical temperature. The Bi, Pb(2223) thermal decomposition temperature for a given oxygen pressure is lowered by at least 10 K by the presence of Ag.

The possibility of controlling Nd-422 phase dimension and morphology, both in the partially melted state and in the final superconducting matrix, was investigated. Nd–Ba–Cu–O samples were prepared by the melt powder melt growth (MPMG) technique. Precursor materials containing Nd as either Nd2O3 or Nd-422, formed during precursor quenching, were used. The role of Pt in Nd-422 refining was analyzed. The effect on Nd-422 nucleation and growth, of stoichiometries with increasing Nd-422 molar excesses (0%, 10%, 20%, and 40%) combined with different heating processes, up to the partially melted state, were examined. Uniformly distributed needle-like particles (1 μm diameter and 10–15 μm length) were obtained at 1120 °C and resulted in a further refined distribution trapped in completely processed samples.

The SiCp/Al nanocomposites were synthesized under high pressure. The reaction behavior between SiC particles and Al matrix within 2–6 GPa pressure range was determined. The high resolution electron microscopy (HREM) observation and the Vickers microhardness measurement show that the reaction is slight and that the adhesion of SiC particles to the Al matrix is good whether the reaction between them occurred or not. This offers an opportunity to tailor the nanocomposite mechanical properties by adjusting the synthesis temperature, pressure, and volume fraction of SiC particles.

A novel metal salt of TCNQ (tetracyanoquinodimethane) has been synthesized via an electrochemical process using cadmium as donor. Thin films of the same material have been obtained by evaporating under high vacuum the metal and the organic molecule. The electronic properties of a pellet of the powdered material have been investigated by means of standard UV-VIS-IR spectroscopy, x-ray photoelectron spectroscopy, and Auger electron spectroscopy. The complex shows two absorption structures at about 3.4 eV and 1.7 eV due to the in-plane intramolecular transitions and a shoulder at about 1.4 eV probably due to the bond with the metal. The infrared spectrum is dominated by a deep absorption structure distinctive of the charge transfer. The electrical conductivity of the sample shows a semiconductor behavior in the investigated temperature range; the best fit of the transport data provides an activation energy of about 0.12 eV and shows that at low temperature the electrical conductivity is mainly due to a hopping process among differently charged sites.

Polysilicon microfracture specimens were fabricated using surface micromachining techniques identical to those used to fabricate microelectromechanical systems (MEMS) devices. The nominal critical J-integral (the critical energy release rate) for crack initiation, Jc, was determined in specimens whose characteristic dimensions were of the same order of magnitude as the grain size of the polysilicon. Jc values ranged from 16 to 62 N/m, approximately a factor of four larger than Jc values reported for single crystal silicon.

A theoretical computation of vibrational anharmonicity is presented which is a generalization of the simple Gruneisen approach. The calculation was based on a model that defines a simple relationship between the binding energy of a solid and the variation of vibration frequencies with volume. The agreement between calculated and experimental Gruneisen constants is good.

Ba(Mg1/3Ta2/3)O3 thin films were prepared by a sol-gel process involving the reaction of barium isopropoxide, tantalum ethoxide, and magnesium acetate in 2-methoxyethanol and subsequently hydrolysis, spin-coating, and heat treatment. Transmission electron microscopy, x-ray diffraction, and Raman spectroscopy were used for the characterization of the thin films. It was shown that the thin films tend to crystallize with small grains sized below 100 nm. Crystalline phase with cubic (disordered) perovskite structure was formed in the samples annealed at a very low temperature (below 500 °C), and well-crystallized thin films were obtained at 700 °C. Although disordered perovskite is dominant in the thin films annealed below 1000 °C, a low volume fraction of 1 : 2 ordering domains was found in the samples and grows with an increase of annealing temperature.

The intermixing and crystallization of amorphous Si/Ge multilayers (with individual layer thickness between 1.5 and 20 nm) and SiGe alloys produced by dc magnetron sputtering have been studied by cross-sectional transmission electron microscopy and x-ray diffraction. Measurement of the crystallization temperature as a function of the Si content showed that multilayers and alloys with equal composition crystallized at the same temperature. This implies that intermixing precedes crystallization in the multilayers. Close to the crystallization temperature, formation of Kirkendall voids was observed in the short-period Si/Ge multilayers. These voids were found at positions corresponding to the original Si layers, indicating that Si diffuses faster in amorphous Ge than Ge in amorphous Si. The Ge layers in short-period Si/Ge multilayers retained their amorphous state to much higher temperatures than thick amorphous Ge layers. This is shown to be due to inhibition of nucleation by the presence of the layer interfaces. A lower estimate for the Si diffusion constant in crystalline Ge is also determined.

The quality and preparation of Sm–Ba–Cu–O (SmBCO) seeds, the level of Pt-doping, and the temperature distribution in the thermal processing system have been investigated in detail and identified as key processing factors in the fabrication of large melt processed Pt dope Y–Ba–Cu–O pseudocrystals. Optimization of these process variables and features has been performed to enable controlled processing of these materials up to several centimeters in diameter. Inhomogeneities and second phases present in the YBCO-Pt pseudocrystal microstructure have been analyzed and correlated with a variation of superconducting properties within the bulk of the sample. These observations have clear implications for the controlled processing of large YBCO-Pt pseudocrystals for electromagnetic applications.

Atomic force microscopy (AFM) is commonly used for microwear/machining studies of materials at very light loads. To understand material removal mechanism on the microscale, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) studies were conducted on the microworn/machined single-crystal silicon. SEM studies of micromachined single-crystal silicon indicate that at light loads material is removed by ploughing. Fine particulate debris is observed at light loads. At higher loads, cutting type and ribbon-like debris were observed. This debris is loose and can be easily removed by scanning with an AFM tip. TEM images of a wear mark generated at 40 μN show bend contours in and around the wear mark, suggesting that there are residual stresses. Dislocations, cracks, or any special features were not observed inside or outside wear marks using plan-view TEM. Therefore, material is mostly removed in a brittle manner or by chipping without major dislocation activity, crack formation, and phase transformation at the surface. However, presence of ribbon-like debris suggests some plastic deformation as well.

Using classical molecular dynamics based on Lennard–Jones-like potentials, a mechanically stable YBa2Cu3O7 high Tc superconductor structure is generated. This process is controlled via interactive computer graphics. After doping atoms into or removing atoms from the sample using a recently implemented picking mechanism, the lattice oscillation energy is annihilated with a simulated annealing procedure. The remaining minimum ground state energy allows marking of the preferred doping location. Information on the doping mechanism is important because the magnetic and superconducting properties of these compounds depend very strongly on their oxygen content.

The strain compensation produced by heavy boron doping in Si1−xGex layers with x = 0.21, 0.26, and 0.34 grown by solid phase epitaxy on (001) Si wafers has been analyzed using high resolution electron microscopy, high resolution x-ray diffractometry, and ion channeling. The structure of the epilayers consists of a defect-free region located next to the layer-substrate interface and a top region which contains strain-relieving defects. In the undoped samples the defect-free layers are partially relaxed and their relaxation increases as the Ge fraction increases. Substitutional boron incorporated to the SiGe lattice to levels of 2.8 ± 0 3 × 1020 cm−3 during the growth process reduces the lattice mismatch between the epilayers and the substrate. The boron-doped, defect-free layers are thicker than the corresponding undoped layers of the same Ge content and their strain relaxation is lower. It has been shown that it is possible to grow at least 27 nm thick defect-free and fully strained heavily boron-doped layers with x = 0.21 by solid phase epitaxy.

Vickers microindentations obtained with loads between 0.05 N and 2 N were performed on crystalline (100) silicon. The residual stress field and the different structural states induced by loading were studied by mapping the indented zones by their micro-Raman response. A Raman signature of amorphous silicon is found in the center of the impression. The energy of the Γ25 zone center phonon is found to vary from 522 cm−1 when probing the silicon at a distance of 80 μm from the center of the indentation up to 527 cm−1 when probing the pileup region of the impression. When probing cracked zones in the vicinity of the pileup region, wave numbers as high as 536 cm−1 are measured. The stress components induced by a point indentation (1 N) have been calculated from analytical expressions given in the literature. For an average conversion factor of 3.2 cm−1/GPa, the residual local stresses after unloading are found of the same order of magnitude or even larger than the calculated stresses that are generated during loading. A tentative explanation is proposed. Finally a systematic laser-induced thermal treatment of the central area and of the pileup region of indentations was performed. It is shown that the amorphous silicon in the center can partly recrystallize but that the residual stress state in the pileup region cannot be completely relaxed by local laser heating.

The phase transformation in Sr1−xBaxNb2O6 (0.25 ≤ x ≤ 0.8) ceramics was investigated. There is an intermediate transitive phase before forming the tungsten bronze phase at higher temperatures. The phase transformation from the intermediate type into tungsten bronze type is sluggish, affected principally by temperature. In the compositions rich in Ba (x > 0.672), Ba ions prefer to occupy the A2 sites rather than the A1 sites of the tungsten bronze structure. The percentages of vacancies in the A1 sites and A2 sites are no longer the same. With the increase of Ba, the vacancies in the A1 sites increase, whereas the vacancies in the A2 sites decrease.

X-ray diffraction line profile analysis (LPA) has been carried out on a set of superconducting thin films of MBa2Cu3O7−δ (MBCO, M = Y, Gd), deposited by pulsed and continuous physical vapor deposition (PVD) techniques on different single-crystal substrates. The choice of appropriate deposition conditions, substrates, and buffer layers promoted a high degree of [00l] preferred orientation, leading to a well-defined columnar grain morphology in the MBCO films. Under such conditions, the LPA of diffraction patterns, collected with the widely spread Bragg–Brentano geometry, gives detailed information on the distributions of coherent scattering domain (crystallite) size and microstrain along the [00l] growth direction; considering the particular MBCO film microstructure, the mean crystallite size () can be regarded as the mean distance between extended planar defects parallel to the film surface. The significance of goes beyond a merely statistical value. As long as the morphology of the films is similar, is found to be strictly connected with the average microstrain by a simple proportionality relation. Moreover, the correlation extends to important superconducting transport parameters, like the transition width ΔTc. These regular behaviors are irrespective of deposition techniques, substrate, and film materials, and are a clear indication of some fundamental relation between the defects and the overall properties of the films.

The origin of a previously reported anomalous low 2θ x-ray diffraction peak from MoS2 thin films grown by ion beam assisted deposition was investigated. The anomalous peak, observed in a film grown on Si(100), was removed by ion irradiating the film with 180 keV Ar++ ions to a dose of 1 × 1015 ions/cm2. Microstructures of the two films were investigated using x-ray diffraction and cross-section transmission electron microscopy. Diffraction data and bright-field images indicated that the low 2θ peak was due to a local interplanar expansion of the crystal structure normal to MoS2 basal planes. This expansion was attributed to molecular defects.

Diamond thin films grown from a dc-arc discharge in CH4/H2 mixtures on Si wafers were examined by transmission electron microscopy and Raman spectroscopy. This deposition method provides good diamond crystallinity at high CH4 concentrations (3%–9%). Seeding the substrate with 5 nm diamond particles at a density of 2 × 1012 cm−1 followed by argon laser irradiation to reduce their agglomeration gives, just after starting deposition, a density of growth centers of 1010cm−2. At 3% CH4 concentration the film grows with almost perfect crystallites. Richer CH4 mixtures (5% and 9%) produce crystallites with twins and stacking faults. An amorphous 20–70 nm SiC interlayer is present at these CH4 concentrations, which was not observed at 3% CH4. Amorphous sp3- and sp2-bonded carbon was detected by Raman spectroscopy at all CH4 concentrations and correlated with TEM data.

It was demonstrated that molten Pd40.5Ni40.5P19 undergoes liquid state phase separation in the undercooling regime δT = T1 − T where T1 is the liquidus of Pd40.5Ni40.5P19 and T is the kinetic crystallization temperature. Liquid state phase separation by nucleation and growth takes place for δT ≤ 60 K while that by spinodal decomposition occurs for δT ≥ 100 K. Microstructural analysis of the undercooled specimen obtained in the undercooling regime of 60 ≤ δT ≤ 100 K indicates that it is the transition regime. Finally, it was found that when undercooled molten Pd40.5Ni40.5P19 undergoes liquid state spinodal decomposition, it first decomposes into two liquid networks, which is finally replaced by a system of three liquid networks.