Two upper critical fields normal (Bc2⊥) and parallel (Bc2∥) to the surfaces of both single-crystal and polycrystalline Nb films are studied at 4.2 K in relation to the purity and morphology of the films, in order to make properties of the single-crystal films clear. High-quality single-crystal Nb films (with transition temperature Tc of ∼9.3 K and normal resistivity ρn of ∼0.2 μΩ · cm) are found to have magnetic properties characterized by Bc2⊥ of 0.31 T as low as Bc2 (bulk upper critical field) of bulk Nb, and Bc2∥/Bc2⊥ of ∼1.85 as high as Bc3/Bc2 (where Bc3 is the surface nucleation critical field) of pure Nb. These properties depend strongly on high purity and surface smoothness of the films, which is naturally accompanied by superconductivity. Polycrystalline Nb films have higher Bc2⊥ and lower Bc2∥/Bc2⊥, which result from a decrease in purity of the films and a presence of normal-conducting niobium-suboxide layers at the surfaces of the films, and thereby a decrease of the surface effect in the films.

Two YBa2Cu3O7−x powders were investigated: one was nearly stoichiometric, and the other, CuO-rich. After being sintered at 950 °C, samples from both powders were heat-treated in oxygen at 845, 860, and 910 °C for up to 10 days. The samples were characterized by differential thermal analysis, x-ray diffraction, optical and scanning electron microscopy, iodometric titrations, and measurement of their superconducting properties (electrical resistivity, critical temperature, and critical current density). The electrical properties of the nearly stoichiometric material improved with time at all temperatures. On the other hand, the electrical properties of the CuO-rich material deteriorated with temperature, possibly owing to problems associated with grain growth at 910 °C.

The role of twinning in deformation and fracture behavior of ordered intermetallic compounds has been investigated from a viewpoint based on the crystallography of twinning. The conjugate relationship between the order twinning and the active slip system at elevated temperatures is identified in all the ordered structures considered. Implications of this conjugate relationship on the strength and ductility of ordered alloys are discussed.

The microstructure of boron-doped Ni3Al powder has been characterized by optical and transmission electron microscopy. Remarkable variations in the solidification morphology and phase reaction were observed as a function of powder size. The degree of boron segregation appeared to be reduced significantly, as the formation of M23B6 boride was suppressed in powder below ∼30 μm diameter. The primary solidification phase was disordered γ–Ni, which underwent a solid-state ordering transition to produce fine γ′–Ni3Al antiphase domains. A bi-modal distribution of domain sizes was observed due to Al segregation. The solidification morphology was dendritic for particles above ∼20 μm, and it changed to cellular below. In powder less than 40 μm diameter, second-phase particles of β–NiAl were found in intergranular regions, likely due to a metastable eutectic reaction of L ⇉ γ + β. The β phase was suppressed only for powder sizes below ∼2 μm. Judging from the tendency of second-phase formation, the Ni3Al–B powder appeared to cool slower than arc-hammer foil and melt-spun ribbon.

Samples of YBa2Cu3O7 were prepared by sol-gel, co-precipitation, and solid state processes. Sol-gel samples were prepared from a solution of yttrium, barium, and copper nitrates dissolved in ethylene glycol, co-precipitated samples were made by the amorphous citrate method, and solid state samples were prepared by conventional high temperature reaction of the appropriate metal oxides and carbonates. The sol-gel process was shown to yield superconducting samples of superior Meissner effect, critical current, and critical field. The co-precipitated samples contain impurities that affect the critical properties. The sol-gel and co-precipitated processes yield materials with well-formed, plate-like particles with a fairly uniform size of about 10 μm. The grains in the solid state sample are smaller but have a much wider distribution of sizes than the samples prepared by solution methods.

Effects of hydrofluoric acid (HF) treatment on the properties of Y–Ba–Cu–O oxides were investigated. No obvious etching of bulk Y–Ba–Cu–O and no degradation of zero resistance temperature were observed even though the oxides were placed into 49% HF solution for up to 20 h. Surface passivation of Y–Ba–Cu–O due to HF immersion was verified by subsequent immersion of Y–Ba–Cu–O in water. A thin layer of amorphous fluoride formed on the surface of the Y–Ba–Cu–O during HF treatment, which limited further reaction between Y–Ba–Cu–O and HF, and later reaction with water. Thin film Y–Ba–Cu–O was passivated by HF vapors and showed no degradation in Tc-zero after 30 min immersion in water. The properties of the surface layer of Y–Ba–Cu–O oxide after HF treatment are reported from Auger electron spectroscopy, x-ray diffraction, and scanning electron microscopy studies.

Alloys of Nb73Al12Si14.5B0.5 were rapidly solidified into amorphous ribbons using the melt spinning technique. These were isothermally annealed at temperatures ranging from 660 to 780 °C. The A15 phase began to crystallize at 700 °C and small amounts of second phases appeared at the higher temperatures. Crystallization was dependent on quenching rate as well as annealing conditions. Below 750 °C nucleation was nonuniform and was enhanced by surfaces and quenched-in nuclei. Above 750 °C nucleation became more uniform and completely crystalline ribbons with equiaxed grains ∼30 nm in diameter were obtained. These ultra fine grained ribbons had extremely high superconducting critical current densities of 8 × 1010 A/m2 and 5 × 1010 A/m2 at magnetic fields of 0.5 and 15 tesla, respectively, at 4.2 K.

Thin films of YBa2Cu3O7−x (YBCO) have been prepared on MgO substrates at 650 °C by rf-planar magnetron sputtering using a single oxide target. Depositions at two different substrate positions were examined: (A) above the inner boundary of the erosion area of a target (position A), (B) right above the center of a target (position B). The films deposited at position A suffered a serious deficiency in the contents of Ba and Cu, especially in the low gas pressure region due to the bombardment of the growing films by high-energy particles. Though we could obtain almost stoichiometric films by raising the gas pressure to 15 Pa to reduce the bombardment, high temperature annealing at 950 °C was required to improve their crystallinity and to achieve high critical temperatures (Tc). On the other hand, those deposited at position B were more excellent in crystallinity than those at position A and showed high Tc above 80 K without any annealing. Critical current density C/r) at 77 K was improved from about 103 A/cm2 to about 104 A/cm2 by annealing at low temperature of 500 °C. It is concluded that the deposition with reduced bombardment by high-energy particles enables the fabrication of high Tc YBCO films without a high temperature process.

This paper describes the effect of grain shape on environmental embrittlement in boron-doped Ni3Al (24 at. % Al). The alloy showed severe embrittlement when tested at 600 and 760 °C in air. The embrittlement can be alleviated by control of grain shape, and the material with a columnar-grained structure produced by directional levitation zone remelting shows good tensile ductilities when tested in oxidizing environments. The columnar-grained structure with vertical grain boundaries minimizes the normal stress and consequently suppresses nucleation and propagation of cracks along the boundaries.

The superconducting properties of the system Bi1−xPbxSrCaCu2Oy have been studied as a function of lead concentration and preparation conditions. Energy dispersive x-ray analysis indicates the nominal stoichiometry is preserved up to x = 0.2 and for this concentration, zero resistance occurs at 97 K. Magnetically modulated microwave absorption measurements provide a global probe of the samples and show that resistance measurements alone can give a false impression of the quality of the materials.

Positron lifetime spectroscopy was used to study the isochronal annealing of cold worked Ni3Al samples. In pure Ni76Al24, Ni74Al26, and boron-doped Ni74Al26 three annealing stages were observed. Boron-doped Ni76Al24 showed only two annealing stages. Vacancy annealing (stage III) was identified in all cases to start at ∼250 °C, somewhat higher than previously reported. The discrepancy is suggested to be due to carbon-vacancy interactions, because carbon (impurities) was observed to diffuse out of all samples at or above ∼350 °C. The high-temperature annealing stage in boron-doped Ni76Al24 (which is ductile) starts at 700–750 °C and is complete at 1000 °C. This stage was attributed to migration of dislocations to various sinks. In pure Ni76Al24, Ni74Al26, and boron-doped Ni74Al26 (which are brittle) the intermediate and high-temperature annealing stages occur at ∼750–800 and 1000 °C, respectively. These stages were attributed to the migration of dislocations (750–800 °C) and recrystallization (∼1000 °C) with incomplete annealing of dislocations at 1000 °C. This being the case, it is clear that dislocations interact with grain boundaries far more strongly in brittle than in ductile Ni3Al alloys. Thus, these data strongly suggest that the ductilization of Ni76Al24 by boron is largely due to a change in grain boundary structure which inhibits the pinning of dislocations at grain boundaries that occurs in pure Ni76Al24 (i.e., boron increases the susceptibility of grain boundaries to slip). Similar results for small-grain samples support this interpretation.

The successful fabrication of ceramic superconducting YBa2Cu3O7−x fibers has been investigated. A new method was proposed for synthesis of the fibers through a solution route. The thermoplastic gels were synthesized using Y, Ba, Cu, ethoxides, and diethylenetriamine. The fibers were drawn from the reheated gels. The fibers were characterized by x-ray diffraction, SEM, and shrinkage ratio measurements. The fired and then annealed fiber is shown to have a superconducting transition temperature of 91 K (onset) and zero resistance temperature of 84 K. With regard to the fired fibers, it is found that the surface area increased and superconducting transition temperature decreased with increasing organic content in the initial gel. The usefulness of this method is shown and the structure of the synthesized gel is discussed.

The pulsed laser deposition technique was used to deposit stoichiometric thin films from multi-component targets. By changing the target during deposition, multilayer thin film structures were fabricated. We have prepared multilayer structures consisting of alternating superconducting layers with different compositions and elements separated by thin insulating layers. The sharpness of the interfaces was studied by Auger spectroscopy depth profiling. Comparison of films deposited at room temperature and at 680 °C showed that a 10 nm yttrium stabilized zirconium oxide film can completely prevent gross interdiffusion between Y–Ba–Cu–O films and between Y–Ba–Cu–O and Si.

Potential and current distributions and local energy dissipation due to Joule heating in metal-superconductor junctions have been computed as a function of geometric parameters and interfacial resistance. The primary current distribution and power dissipation are highly nonuniform in the system. The secondary current distribution and power dissipation, however, become more uniform as the interfacial resistance increases. Analysis indicates that zero contact resistance is not a stable situation since the primary distribution leads to local current densities exceeding the critical current density of the superconducting phase near the corner of the junction. Local contact failure might then initiate. A finite contact resistance is necessary for a practical application, and the minimum value of the contact resistance can be estimated from the operating current density (javg) of the device and the critical current density (jcri) of the superconducting phase. To obtain an optimum value of the contact resistance, however, one further has to take into consideration the stability and reliability of the device performance, which is, in turn, directly related to the uniformity of the current distribution and power dissipation, to temperature fluctuation of the superconducting phases brought about by local power dissipation, and to the thermal management of the system. Furthermore, a nonuniform contact resistance layer of appropriate profile can redistribute the current more effectively and more uniformly and hence reduce the total power dissipation in the system for a given jmax/javg ratio obtained by a uniform resistance layer.

Combinations of inert atmosphere sintering and oxygen atmosphere sintering have previously been reported as necessary for the synthesis of LaBa2Cu3Oy superconductors which achieve zero resistance at temperatures above 90 K. Sintering under oxygen atmosphere only is known to produce La(1+x)Ba(2−x)Cu3Oy, in which La is substituted for Ba in the crystal lattice. The latter substituted compounds achieve zero resistance at temperatures well below the boiling point of liquid nitrogen. In this work, we show that during the initial inert atmosphere sintering step, LaBa2Cu3Oy powder decomposes, in part, into several intermediate compounds. These compounds are then recombined in the subsequent oxygen atmosphere sintering step to form LaBa2Cu3Oy, which achieves zero resistance at temperatures above 90 K. We propose that the net effect of these two processing steps is to inhibit the substitution of La for Ba in the lattice of the fully processed material.

Iron-chromium-phosphorus (Fe–Cr–P) alloys were prepared by electrodeposition from an acidic citrate electrolyte using sodium hypophosphite as the source of phosphorus. These alloys form a passive oxide layer when exposed to air and are useful as protective coatings on steel. The current efficiency of the plating process reaches a maximum of 20% at a current density of 100 mA/cm2 where the alloy has 10% Cr and 19% P. X-ray diffraction patterns and TEM analysis show that the alloy is amorphous. TEM results also indicate that small oxide particles (5–20 nm) are dispersed in the amorphous structure. Besides Fe, Cr, and P, the alloys contain a low level of oxygen (4–7%) in the form of mixed iron and chromium oxides, as confirmed by AES analysis. When heated, the amorphous structure transforms into a mixture of Fe3P and Cr3P, along with α–Fe–Cr grains. This phase transformation occurs in the temperature range of 450–460 °C for alloys with 19% P.

A nucleation-and-growth mechanism for the twin formation in YBa2Cu3O7–δ superconductors based on the oxygen uptake rate curve and published transmission electron microscopic observations is proposed together with an oxygen-depleted twin boundary model. The difficulty of reaching stoichiometric YBa2Cu3O7 is explained.

Twin roller quenching from the melt at cooling rates of ∼107 K s−1 was used on several Bi-containing high Tc compositions. Pure glass was obtained in most compositions and the route of crystallization was studied by differential thermal and thermogravimetric analysis, x-ray diffraction, and magnetic measurements. Heating of the glasses produced poorly crystallized short-range-order-only as determined by x-ray diffraction, despite passing through several exotherms, some of which were very strong. This anomalous behavior deserves further investigation. On heating to higher temperatures the expected double-copper-oxide-layer high Tc phase formed sluggishly via intermediate CuBi2O4 and/or single-copper-oxide-layer Bi2(Sr, Cu)2CuO4 phases. Considerable oxygen absorption of about 0.5 O per Cu occurs during these steps, peaking at about 680 °C; some of this oxygen is lost again by the time the high Tc phase forms just below the melting point.

We have used “local volume” (embedded atom) type potentials to study the surfaces and grain boundaries of Ni, Al, and Ni3Al. The simulations show that with appropriately fit potentials, the surface and grain boundary structure can be realistically calculated. The surface rippling and relaxation show good agreement with experiments. The energies of most surfaces and grain boundaries also agree with existing data. The structural unit model for grain boundaries in Ni3Al shows the same generic units as in pure metals, but with large variations due to distortions and multiplicity. The utility of the structural unit model is thus more limited for alloys. The grain boundary energies were found to be the highest for Al-rich Ni3Al grain boundaries, and depend significantly on the local composition of the grain boundary. The cusps in the grain boundary energy as a function of misorientation angle are different for different grain boundary stoichiometries. The Ni3Al grain boundaries have approximately the same grain boundary energy and cohesive energy as that of Ni.

Rapidly solidified Al–Cr alloys up to 20 at. % Cr were studied to delineate the extent of crystalline and quasicrystalline phase formation in these alloys in comparison with as-cast alloys by using transmission electron microscopy and x-ray diffraction technique. The icosahedral quasicrystals are observed from 7 to 15 at. % Cr alloys, while equilibrium η–Al11Cr2 phase is completely absent. Both rapid solidification and subsequent thermal decomposition studies indicate that the main competing phase is θ–Al2Cr up to 15 at. % Cr. Beyond this composition ∊–Al4Cr is the dominant phase together with a small amount of γ4–Al7Cr3. We have shown that the electron diffraction patterns of Al–Cr quasicrystals are often associated with a diffuse intensity distribution, indicative of short-range order. The change in quasilattice constant with composition suggests the existence of structural vacancies. Further, a sudden change from coarse to ultrafine quasicrystalline grain structure in Al-7 at. % Cr alloy points to a change in nucleation mechanism from heterogeneous to homogeneous mode during the rapid solidification.