Y-Ba-Cu-O films were made by R-F diode sputtering using a single oxide target. It was found that if a small negative bias is applied to the substrate, the etching associated with reactive sputtering is significantly reduced. This results in better composition control and uniformity, which are quite important for the formation of superconducting thin films. Films deposited on strontium titanate, when annealed in oxygen, become superconducting with zero resistance at 89 K.

Yttria stabilized zirconia powder was synthesized by aerosol pyrolysis of an Y-Zr-nitrate solution. The particles were spherical and had a narrow size distribution, peaking at 0.4 μm. Material made by this process is phase-pure (cubic) and has high chemical purity.

Preparation of the superconducting oxide, YBa2Cu3O7−x, was carried out according to the metal alkoxide method. To obtain a homogeneous solution of yttrium, barium, and copper alkoxide in an organic solvent, alkoxides of copper and yttrium were modified by the O-R interchange reaction with 2-dimethylaminoethanol and the structures of their modified alkoxides were studied by 1H-NMR, FT-IR, and EXAFS. The YBa2Cu3O7−x precursor, prepared by hydrolysis of the present solution of alkoxides, was calcined at 850°C for 3 h to give YBa2Cu3O7−x powder as a single phase. This powder was sintered between 900°C and 950°C and characterized for bulk density, microstructure, Tc, and Jc.

We studied the electrical current induced superconducting-resistive transitions in laser deposited c-axis oriented crystalline Y1Ba2Cu3O7−x superconducting thin films. Comparative studies of I-V characteristics of thin film bridges with different geometries at temperatures below Tc and SEM voltage imaging of current induced resistive regions in the same samples were performed. The I-V curves of these bridges had two nonlinear regimes, a gradual and an abrupt transition to the normal state. We concluded that the gradual nonlinear transition is caused by imperfections in the sample such as film and substrate defects, film thickness variation, etc., and by dissipative effects such as flux motion and superconductor/normal-metal/superconductor type behavior. The abrupt transition to the normal state in the I-V curve is ascribed to Joule heating. The SEM mapping provides a direct image of the above effects and is useful for material or device characterization and for studying the transport properties of high Tc films.

Structural defects in thin films of nominal composition YBa2Cu3O7 (123) grown on single crystal MgO have been characterized. The main types of stacking defects correspond to the cationic stoichiometries of “248”, “247”, and “224”. Several types of edge dislocations have been observed. Due to the frequent changes in the stacking sequence, antiphase boundaries are created to accommodate the misfit across regions in which the repeat sequence is not identical. The films exhibit a mosaic microstructure due to the formation of grain boundaries in the a-b plane.

As-deposited superconducting Y-Ba-Cu-O films have been grown on stainless steel substrates by the plasma assisted laser deposition technique. Low interfacial diffusion of iron at the 550°C growth temperature enables us to produce superconducting films with critical temperatures up to 83 K and critical currents up to ∼4 × 103 A/cm2 (40 K). Dependence of the superconducting properties of the Y-Ba-Cu-O films on the surface condition of the mirror finished stainless steel substrate has been studied. Critical temperature and critical current of the films have been improved by heat-treating the substrate and incorporating buffer layers. Variation of the critical current with the bend radii of the film is discussed.

Samples of Y-Ba-Cu-O materials with the formulation Y:Ba:Cu = x:2:3 and values of x ranging between 1 and 3 were prepared by partial melting at a maximum temperature of 1045 °C. Measurements of magnetic susceptibility and maximum (low-field) as well as remanent magnetization show highest values for x = 2. XRD and SEM/EDX analyses show that the corresponding structure involves numerous small crystals of Y2BaCuO5 (211) embedded in highly ordered assemblages of continuous YBa2Cu3O7−y (123) layers. The presence of these impurity sites is correlated with flux pinning capacity. Other impurity phases include CuO, a minor phase which shows an increase in amount when x increases, BaCuO3, a possibly detrimental minor phase which vanishes when x is raised from 1 to 2, and zones of intermediate composition between the 211 grains and the 123 layers, which are formed from the residual liquid upon cooling. These intermediate regions, like the 211 grains themselves, become gradually more important when x is increased from 1 to 3.

Using both x-ray and electron diffraction, we have studied the incommensurate modulation structure in single crystal Bi2Sr2CaCu2Ox. Electron diffraction clearly indicates a small a∗-axis component of the modulation wave vector k, along with the more familiar b∗-axis component (0.004a∗ + 0.212b∗). This tilt of the k-vector breaks the mirror symmetry perpendicular to a- and b-axes as well as the twofold symmetry about a- and b-axes. The modulated structure thereby has only a mirror plane normal to the c-axis. Intense x-ray streaking along the c-axis at several satcllite reflections was considerably more pronounced than at the fundamental reflections, indicating a stacking disorder along the c-axis predominantly in the modulated structure.

Chemical compositions of superconductors of Bi1−xPbxSrCaCu1.8Oy (x = 0.1, 0.3, and 0.5) were investigated by analytical electron microscopy (AEM) supplemented by electron microprobe analysis. Samples were prepared by a solid state reaction method under oxygen partial pressures of 0.20 and 0.077 atm. The high-Tc phase appeared only in the samples of Bi1−xPbxSrCaCu1.8Oy (x = 0.1 and 0.3) prepared under an oxygen partial pressure of 0.077 atm. In the samples containing the high-Tc phase, stacking structures of 2, 3, and 4 perovskite layers were observed by transmission electron microscopy (TEM). From AEM analysis, it was shown that in order to make the high-Tc phase, the substitution ratio of Pb for Bi was about 0.2.

XRD shows that doping BaBiO3 with alkali ions transforms the larger monoclinic parent lattice into a more compact cubic or nearly cubic lattice. This lattice contraction favors the transition from semiconductor to metal. It leads also to superconductivity. Doping BaBiO3 with both K and Rb raises the onset resistivity Tc above those obtained by doping with either K or Rb.

We describe a low-temperature solid-state interdiffusion technique that allows reaction between spatially separated reacting species and its application in the Al–Ru alloy system. This technique uses a liquid-metal solvent (Bi) as a medium for the transfer of Al to the surface of Ru powder where reaction occurs with the formation of nanocrystalline AlxRu1−x product phases. X-ray diffraction measurements are used to follow the time and temperature dependence of the reaction. Cross-sectional transmission electron microscopy allows direct imaging of the growth and morphology of the AlxRu1−x product phases.

The room-temperature tensile properties, fracture mode, and grain boundary chemistry of undoped stoichiometric NiAl, as well as NiAl doped with boron, carbon, and beryllium, have been investigated, Pure, stoichiometric NiAl fractures with limited tensile ductility in a predominantly intergranular manner. Auger analyses revealed that the grain boundaries in NiAl are extremely clean and free of any segregated impurities, indicating that they are intrinsically brittle. Boron, when added to stoichiometric NiAl at a bulk level of 300 wt. ppm, segregates to the grain boundaries and suppresses intergranular fracture. However, there is no attendant improvement in tensile ductility because boron is an extremely potent solid solution strengthener in NiAl, more than doubling its yield strength. As a result, any potential benefit of improving grain boundary strength is more than offset by the increase in yield strength. Unlike boron, both carbon (300 ppm) and beryllium (500 ppm) are ineffective in suppressing intergranular fracture in NiAl, and Auger analyses of the C-doped alloy revealed that carbon did not affect the fracture mode because it did not segregate to the grain boundaries. Although neither beryllium nor carbon suppressed grain boundary fracture, their effects on the tensile ductility of NiAl were quite different: the ductility of the Be-doped alloy was higher than that of the B-doped alloy because beryllium, unlike boron, has a rather modest strengthening effect in NiAl, whereas the C-doped alloy was brittle like the B-doped alloy, because carbon is a potent solid solution strengthener, just like boron. These observations were rationalized by considering a hard-sphere model for interstitial and substitutional sites in NiAl. It was concluded that boron and carbon occupy interstitial sites, whereas beryllium dissolves substitutionally. In all the alloys that were investigated, the Ni and Al contents of the grain boundaries were not significantly different from the bulk levels, and no evidence was found for B–Ni cosegregation.

An x-ray powder diffraction method was used to determine the location of tantalum atoms in Ni3Al. A series of Ni3(Al, Ta) alloys were produced with tantalum contents ranging from 0.1 to 3.0 at.%. Fine powders with average particle sizes less than 80 μm were made from melt-spun ribbons by a grinding process. The values of the intensity of the (100) superlattice peak normalized to that of the (200) fundamental peak as a function of tantalum content agreed with the calculated values, assuming that tantalum atoms substitute on aluminum sites, not on nickel sites, and also assuming small amounts of anti-site defects exist in the ordered fee structure of Ni3(Al, Ta) alloys. It is concluded from our experiments that tantalum atoms substitute for aluminum in Ni3Al. The long-range order parameters thus calculated of the Ni3(Al, Ta) alloys are generally above 0.84 and below 0.95, except for Ni75Al24.8Ta0.2, at which composition the long-range order parameter is close to unity.

Differential scanning calorimetry and transmission electron microscopy have been used to study thermal fatigue due to diffusionless phase transformation cycling in pure cobalt. Thermal cycling through the allotropic (hcp ↔ fcc) transformation results in a temperature shift of the calorimetric peaks, which means a delay of the transformation. In addition, the transformation enthalpy, which is greater on heating than on cooling, diminishes when the number of transformation cycles increases. This is interpreted as being due to an evolution of the microstructure. Transmission electron microscopy shows the appearance of transformation-induced defects, which are mainly sessile dislocations. We can interpret the calorimetry results (enthalpy evolution and transformation delay) as due to the interactions between interface dislocations and these sessile dislocations.

Continuous indentation testing was used to measure the hardness as a function of indentation depth, of three micron thick copper films deposited on silicon with an intermediate layer of 20 nm thick chromium or titanium. Three different indenters, a nearly perfect Vickers, a Vickers with a 1.2 μm2 flat, and a Pyramid with a 25 μm2 flat were employed. The hardness data suggest that the titanium interlayer produced significantly greater film/substrate adhesion than the chromium interlayer. A compressive residual stress, which relaxed with time, was detected in the samples with the titanium interlayer.

We have studied the structure of Bi films grown on BaF2 substrates as a function of the distance from the interface with the substrate. Close to the interface the films show a polycrystalline structure and probably contain some amorphous regions. The crystallite size increases as the distance from the interface increases. At distances ≥90 nm the film becomes single crystalline and has the (111) trigonal direction normal to the film surface. Our structural data relate very well to mobility measurements performed on samples grown under the same conditions. Our results suggest that the carrier mobility is higher at distances ≥90 nm from the interface, where the film is single crystalline, than close to the interface, where it is polycrystalline.

Recently there has been an emphasis on the importance of using cooling scans in DSC experiments in studying the glass transformation kinetics of glasses. The physical interpretation of the apparent activation energy from DSC heating scans has been questioned as not being meaningful. The present paper reports glass transition temperature (Tg) measurements derived from Differential Scanning Calorimetry (DSC) experiments on bulk and film amorphous selenium samples subjected to heating, at constant rate r, and cooling, at constant rate q, scans. Film samples were prepared by thermal evaporation techniques in vacuum. It is shown that for both bulk and film forms of a–Se, within experimental errors, log(r/T2gm) vs 1/Tgm plot where Tgm is the peak glass transformation temperature, and log(r) vs 1/Tgh plot, where Tgh is the glass transition onset temperature from DSC heating scans, are parallel to the log(q) vs 1/Tgc plot where Tgc is the glass transition temperature from cooling scans. Within the Hutchinson and Kovacs formulation of the glass transformation phenomenon, the results imply that the structural contribution to the mean retardation time, τ, is negligible in comparison with the temperature dependent part. The mean structural relaxation time for both bulk and film forms was found to exhibit a typical Vogel-Tammann-Fulcher type of temperature dependence. Furthermore, the structural relaxation rate was observed to be inversely proportional to the viscosity, η(T), implying that the mean structural retardation time is proportional to the viscosity, τ ∼ η. The results also confirm that the earlier studies of glass transformation kinetics in a–Se utilizing only DSC heating scans remain meaningful.

Silicone gels are becoming more accepted as protective coatings for Very Large Scale Integrated circuits (VLSI) against severe environments due to their excellent electrical, thermal, and mechanical properties. Recent studies indicate that high performance silicone gels in low-cost, non-hermetic plastic packaging may replace conventional hermetic ceramic packaging. This paper describes the use of the soft silicone gels as coatings on Integrated Circuit (IC) devices, and the correlation between the material's cure temperature and cure time versus their adhesion and electrical reliability during 85°C, 85% RH and bias accelerating testing. In addition, the reaction kinetics of the silicone gel based on the Differential Scanning Calorimetry (DSC) study of the uncured sample will be reported.

Thin carbon films grown from a low pressure methane-hydrogen gas mixture by microwave plasma enhanced CVD have been examined by electron microscopy. Previously reported transmission electron microscopy (TEM) of the diamond films has shown that the majority of diamond crystals have a very high defect density comprised of {111} twins, {111} stacking faults, and dislocations. In this study, high resolution electron microscopy (HREM) has been utilized to lattice image individual defects in these polycrystalline diamond films. Interpretation of the images from these defects is not trivial and reported image simulations have been utilized to understand further these defects. Fivefold multiply twinned particles have also been examined and it was found that the 7.5° misfit present in such particles has been accommodated at the twin boundaries rather than by elastic deformation. This creates a twin boundary coincident with a low angle grain boundary which has been termed a “tilted twin boundary”. The density of defects in these particles is generally high; however, a dramatic reduction in the defect density near the twin boundaries was observed. This defect reduction is significant because if its origin can be determined, this information may be useful in producing higher quality diamond films.

Results of room-temperature optical studies on ∼10 micron thick, free-standing diamond films are reported. The films were grown on Si(100) substrates by hot filament-assisted chemical vapor deposition (CVD) from a methane/hydrogen mixture. The as-grown, free surface of the films exhibited a surface roughness of scale σ ∼ 0.2 to 5 microns, depending on the methane/hydrogen mixture, which introduces significant optical scattering loss for frequencies greater than 0.5 eV. Specular reflection and transmission spectra in the range 0.01–10 eV were collected. Below the threshold for interband adsorption near ∼5 eV, the films studied behaved approximately as thin parallel plates of refractive index 2.4, with the rough free surface leading to increasingly larger loss of specular transmission/reflection with decreasing wavelength. Structure in the mid-infrared transmission spectra was observed and attributed to disorder-induced one-phonon absorption, intrinsic multi-phonon absorption, and infrared active –C–H2 stretching modes. The strength of the C–H band was observed to increase with increasing methane pressure in the growth chamber. At 5.3 eV, the onset of interband absorption was observed, in good agreement with the value of the indirect bandgap in type IIa (intrinsic) diamond.