Prolonged exposure of chemical vapor deposited, polycrystalline ZnSe to high ac voltages in the presence of a 1 molal NaCl solution induces severe mechanical damage. The damage takes the form of defects which originate at the surface and grow intergranularly into the bulk with a bush-like morphology. Neither exposure to the salt solution in the absence of the high voltage nor low voltage dc electrolytic exposure produces the defects. The damage may be associated with an intergranular hydride phase or grain boundary impurity segregations present or formed during the environmental exposure.

Metal-organic precursors can facilitate the production of superconducting thin films on large area substrates for microelectronic device applications. This paper describes the chemistry that occurs during the thermal processing of yttrium-, barium-, and copper-neodecanoate mixtures into a superconducting material, YBa2Cu3O7−x. Intermediates such as metal carbonates and oxides are identified by combining thermogravimetry with infrared spectral and x-ray diffraction analysis. Changing from argon to oxygen atmospheres increased decomposition rates and metal oxide formation. We found that (1) a low temperature (500–600 °C) decomposition in an oxygen-poor atmosphere, (2) a high temperature (>925 °C) annealing step in an oxygen-rich atmosphere, and (3) slow cooling to 50 °C are all required to produce uniform superconducting films.

GdBa2Cu3O7 crystals were irradiated at room temperature with 200 keV Ne ions and 300 keV Xe ions. In situ standard TEM and further HREM studies show two types of extended defects: (i) mobile extended defects, which account for the preferential defect pinning to twin boundaries reported earlier. These defects are rapidly recovered and difficult to observe by HREM investigations; (ii) stable amorphous areas which are clearly identified by HREM observations. Their overlapping and aggregation conceivably lead to amorphization of the sample.

Growth conditions for YBaCuO thin films are investigated. Films have been made by reactive e-beam coevaporation using three metal sources. In the best cases, as-made films are superconducting with Tc's (R = 0) up to 90 K and Jc's (at 4.2 K) above 107 A/cm2. Oxygen pressure, deposition temperature, as well as compositional dependencies of the films are presented. It is found that in conditions of lower oxygen, pressure films with average composition off the 1–2–3 stoichiometry have higher Tc's. For pressure <10 mTorr, the highest Tc obtained is for Ba/Y deposition ratio ⋚1.4. The morphology and impurity phases of these films are examined. The Ba-deficient films have oriented CuYO2 and CuO as the dominant impurity phases. C-axis lattice parameters (c0) are also examined. It is found that for a given Tc, films made at lower pressure have c0's which are expanded compared to the films made at higher pressures (>100 mTorr). The expanded c0's for these films cannot be reduced by a low temperature oxygen anneal. We suggest that metal-atom point-like defects are quenched into these films and we discuss a particular Ba-for-Y substitution model.

Powder x-ray diffraction, d.c. and a.c. susceptibilities, and SEM have been used to study (Bi1−xPbx)2Sr2Ca2Cu3O10−δ fibers grown by the Laser Floating Zone method. The well-oriented, long-grained superconductor fiber properties are shown to be highly dependent on the partial pressure of oxygen in the growth atmosphere, as well as on fiber pulling rate. Slowly grown fibers contain initially the 2212 (80 K) phase; the 2223 (110 K) phase also appears upon annealing in air. Faster growth rates result in fibers that contain a mixture of the 2212 and 2201 phases and, in this case, long annealing procedures are necessary to observe the 2223 phase.

Superconducting Y1Ba2Cu3O7−δ films were prepared on the MgO (100) and SrTiO3 (100) single crystals using metal organic chemical vapor deposition (MOCVD) of β-diketone metal chelates of Y(thd)3, Ba(th)2, and Cu(thd)2. The evaporation kinetics of Y(thd)3, Ba(thd)2, and Cu(thd)2 and the ratios of deposited to evaporated mole percents of Y, Ba, and Cu cations were studied. The microstructure of Y1Ba2Cu3O7−δ films deposited using MOCVD was observed using scanning electron microscopy and transmission electron microscopy to investigate surface morphology change with the film composition and transformation twin structures. The experimental results showed that the volatility of Ba(thd)2 did not perceptively increase with decreasing evaporation pressure from 10 Torr to 5 Torr, but that of Y(thd)3 or Cu(thd)2 increased with the pressure decrease. The ratio of deposited to evaporated mole percents of Ba cation was smaller than those of Y and Cu cations. Therefore, Ba must be evaporated more than the stoichiometric amount for Y1Ba2Cu3O7−δ in order to obtain single phase Y1Ba2Cu3O7−δ films. The surface morphology of the Y1Ba2Cu3O7−δ films showed perculiar changes with slight composition changes. The transition onset and zero resistance temperatures of typical stoichiometric film deposited on MgO were 93 K and 91 K, respectively. The Y1Ba2Cu3O7−δ films had about 50 nm grain size, and most grains consisted of transformation twins. The critical current density of a film deposited on SrTiO3 was 105 A/cm2 at 77 K and zero magnetic field.

An x-ray diffractogram was generated from a powder sample of solution treated and ice brine quenched Al–14.25 at.% Li alloy. The Bragg reflections obtained were characteristic of a very-nearly fully ordered Al-rich L12 phase based on δ'Al3Li together with two very weak reflections associated with δAlLi. All the lines were significantly broadened due to particle size effects. The average particle size associated with the 100 L12 superlattice line was found to be 4.2 (3) nm and with the fundamental lines, 26.8 nm. A simple structure factor calculation indicated the volume fraction of ordered phase to be around 0.77, assuming that the lack of maximum order was due to the presence of disordered fcc AlLi solid solution. These results suggest that the microstructure of this as-quenched alloy comprises ordered regions of about 4 nm in size in a sea of disordered matrix with a very small amount of δAlLi present. This conclusion is in excellent agreement with recent small angle x-ray and transmission electron microscope studies on similar alloys and suggests that AlLi alloys which are ostensibly disordered at high temperatures go through a disorder-order transformation and then decompose into regions of order and disorder which are associated with a composition spinodal.

The mechanism underlying the hydrogen-induced embrittlement effect in FeAl has been investigated using a local density functional total-energy approach. The bonding characteristics, the bond and cleavage strength between iron and aluminum layers, and the surface energy with and without interstitially absorbed H are calculated from first-principles band-structure and atomic-cluster methods. Our unique combination of techniques permits the simultaneous study of the metallic and localized bonding effects on an equal footing. Results from this study show that FeAl (in the absence of H) is intrinsically highly resistant to cleavage fracture in terms of the high theoretical cleavage strength. Hydrogen locally dilates the Fe–Al lattice, and this is accompanied by a sizable decrease in Fe–Al cleavage (or cohesive) strength. Our results suggest that the underlying mechanism of H-embrittlement in aluminides is a depletion of d-bonding charge on the Fe site resulting from the charge transfer from Fe to H. Results also indicate that the H-embrittlement effect is greater for H adsorbed in Fe-rich sites.

Electron microscope studies have shown significant changes in the microstructure of the Nd14Fe80B6 melt-spun ribbons, depending on the quenching conditions. The average grain size of about 20 nm near the wheel side, increasing to 500–700 nm near the free side, can be observed for ribbons of the thickness of about 25–30 μm, indicating strong internal variations in quench rate across the ribbon thickness. For low quenching rates different morphologies of the crystalline phase Nd2Fe14B are observed. Equiaxed grains near the wheel side of the ribbon become columnar grains or even dendritic grains near the free side. Texturing effects in the equiaxed grains are observed only for grains larger than 30 nm and disappear for very large equiaxed grains (about 500 nm), as well as for dendritic structures. Most evident texture is observed in columnar grains, which crystallized with the c-axis perpendicular to the ribbon plane.

A simple analytical model for the effect of mechanical strength and line width (for the case of narrow lines) on the electromigration failure of metallic interconnects is presented. Because the line width/grain size ratio and the diffusivity enter differently in the model, application of the resulting failure time equation to published data can provide insight into the mechanisms of enhancement of electromigration resistance by grain structure optimization and alloying.

Molybdenum nanocrystals (4 nm < particle size < 12 nm) were synthesized in the vapor by sputtering in a thermal gradient at argon pressures between 0.2 and 0.6 Torr. The gradient was achieved by cooling the substrate table with liquid nitrogen in order to enhance the deposition rate of the nanocrystals. The size of these nanocrystals depended on the sputtering argon gas pressure. Using appropriate deposition parameters, these nanocrystals were incorporated, either as a dispersed phase in a major phase produced by normal sputtering or as a layer in a layered structure to produce nanocomposite films. Results of Auger electron spectroscopy (AES) study of the Al/Mo layered nanocomposite films are presented. The Knoop microhardness of these films was increased by as much as a factor of four compared with the hardness of homogeneous Al films. A correlation of the microhardness to the microstructures as revealed by transmission electron microscopy (TEM) is discussed.

A technique has been developed to measure the surface tension of thin foils under their own vapor pressure. The zero creep method of surface tension measurement is used in conjunction with laser interferometry. This technique allows very small sample strains to be measured. Sample length changes of the order of 0.3 μm were measured with the laser interferometer. The sensitivity of the laser interferometer/zero creep system allows the surface tension to be measured much closer to the Tammann temperature, which is approximately one-half the melting temperature (≍1/2 Tm) of the material. The system has been tested on thin Sn foils in air, and on thin Al and Ni foils under their own vapor pressure (vacuum).

Alloy films of Ni–Co and Ni–Cr of compositional ratios 1:1, 1:3, and 3:1 deposited by vapor deposition were studied by Transmission Electron Microscopy (TEM) and X-Ray Diffraction (XRD). Results of TEM analysis on the Ni–Co alloy films indicated that the films were face-centered cubic (fcc) in structure. XRD results confirmed the TEM observations. TEM analysis of Ni–Cr alloy films showed that the films were body-centered cubic (bcc) in structure. With increase in the Cr content more than 25%, the material contained a higher fraction of an amorphous phase. XRD studies provide limited information owing to the quasi-amorphous structure of the films of high Cr content.

The microstructure of two metastable crystalline phases, which are formed during the first step of the crystallization process in Ni–Zr metallic glasses, was investigated by transmission electron microscopy. For the composition Ni33Zr67, crystallites with average size of 150 nm having the face-centered cubic E93 structure are formed. For the Ni42Zr58 composition, 100 nm size crystallites with a simple cubic unit cell, space group Pa3 are formed. The microstructure of the crystallites in the early stage of crystallization of the two phases is similar to globular morphology and internal striations.

A highly effective wetting agent and emulsifier, Triton X-100 detergent is introduced to metalorganic solutions. When applied to a substrate, this detergent/metalorganic solution promotes the formation of a uniform spin-on thin film with good adhesion. The precursor, copper formate film, was spin-deposited with a metalorganic solution prepared by a solvent mixture of methanol and Triton X-100 (50:1 by volume). KrF laser (248 nm) direct writing of high-purity copper patterns on glass and polyimide substrates has been achieved. When the laser beam is imaged through a slit device, periodic copper metal structures with a linewidth of ∼2.5 μm are observed, which may be attributed to result from Fraunhofer diffraction. A general process for casting homogeneous amorphous films on substrates from a solution of molecular or ionic metalorganics dissolved in the neutral or charged micelles is proposed.

Copper compounds of different chemical compositions and particle shapes were prepared by homogeneous precipitation from copper salt solutions in the presence of urea. It was demonstrated that the nature of the anions played an essential role in the properties of the generated solid phase. Thus, Cu(II)-nitrate solutions yielded spherical amorphous particles which had the composition of malachite [Cu2(OH)2CO3], the Cu(II)-chloride solutions gave bipyramidal particles of atacamite [CuCl2 · 3Cu(OH)2], and in Cu(II)-sulfate solutions needle-shaped brochantite [3Cu(OH)2 · CuSO4] or platelets of posnjakite [3Cu(OH)2 · CuSO4 · H2O] were formed. The addition of NaOH to prepared dispersions resulted in a rapid phase transformation of all above solids into needle-like Cu(OH)2. Calcination of various copper basic compounds at 700–800 °C temperature produced CuO, while the particle morphology was retained.

The transport properties of isotropic pitch-based carbon fibers with surface area 1000 m2/g have been investigated. We report preliminary results on the electrical conductivity, the magnetoresistance, the thermal conductivity, and the thermopower of these fibers as a function of temperature. Comparisons are made to transport properties of other disordered carbons.

Surface planarity and epi/SiO2 interface characteristics of selective epitaxial growth (SEG) and epitaxial lateral overgrowth (ELO), deposited at 800–950 °C/10 or 25 Torr, have been studied for micron-sized structures. SEG at 860 °C showed superior planarity and reduced ratio of facet width to epi thickness, compared to higher deposition temperatures. Data showed that epi/SiO2 interface defects are greatly reduced for structures parallel to (100) and/or by adding HCl to the source gas, compared to interfaces positioned at standard orientation (110) on a (100) substrate. The transition from SEG to ELO in view of the facet orientations will be discussed. To correlate structural with electrical data, n+/p diodes were fabricated on as-grown and polish planarized SEG. Leakage current values of approximately 100 nA/cm2 could be measured. These are comparable to similar n+/p junctions fabricated on conventional epi.

Conventional and high resolution electron microscopy (HREM) were used to study the structure of {113} defects in high-dose oxygen implanted silicon. The defects are created with a density of 1011 cm−2 below the buried oxide layer in the substrate region. The HREM images of the {113} defects are similar to the ribbon-like defects in bulk silicon. It is proposed that there is a third possible structure of the defects, in addition to coesite and/or hexagonal structures. Portions of some defects exhibit the original cubic diamond structure which is twinned across {115} planes. The atomic model shows that the {115} interface is a coherent interface with alternating five- and seven-membered rings and no dangling bonds.

Solid state reactions between SiC ceramics and Co, Ni, and Pt metals have been studied at temperatures between 800 and 1200 °C for various times under He or vacuum conditions. Reactions between the metals and SiC were extensive above 900 °C. Various metal silicides and carbon precipitates were formed in layered reaction zones. Interfacial melting was also observed at certain temperatures; teardrop-shaped reaction zones, porosity, and dendritic microstructure resulting from melting/solidification were evident. The metal/ceramic interfaces exhibited either planar or nonplanar morphologies, depending upon the nature of the metal/ceramic reactions. Concave interfacial contours were observed when interfacial melting occurred. By contrast, planar interfaces were observed in the absence of interfacial melting. In all cases, the decomposition of SiC was sluggish and may serve as a rate limiting step for metal/ceramic reactions. Free unreacted carbon precipitates were formed in all the reaction zones and the precipitation behavior was dependent upon the metal system as well as the location with respect to the SiC reaction interface. Modulated carbon bands, randomly scattered carbon precipitates, and/or carbon-denuded bands were formed in many of the reaction zones, and the carbon existed in a mixed state containing both amorphous and graphitic forms.