Critical current density and microstructure of YBa2Cu3O7 thin films post-annealed at a low oxygen partial pressure

Post-annealing of thin films of YBa₂Cu₃O₇ (YBCO) has been performed at 29 Pa and 750°C. For films 0.6 m thick, a critical current density >1 MA cm^–2 is obtained at 77 K, with a sharp eddy current response at 25 MHz. Microstructural investigation of these films by crosssectional and planar transmission electron microscopy reveals that the YBCO film has thec-axis normal to the plane of the substrate in a continuous sheet of varying thickness, frequently covering the entire thickness of the film. Mutually perpendicular rods with thec-axis in the plane of the LaAlO₃ substrate are also seen. The microstructure and critical current density of these films are compared with those of previously reported films post-annealed in atmosphericpressure oxygen.     

Reproducibility of transition temperature and critical current density of thin films of YBa2Cu3O7 on (100) LaAlO3

Submicrometer epitaxial films of YBa₂Cu₃O₇(YBCO) on (100) LaAlO₃ were made by coevaporation and furnace annealing. Samples from more than a dozen runs are used in this study. The zero resistance transition temperature (T _c) is high (89 or 90 K) if the film composition is phase pure (Ba/Y=2, Cu/Y=3) or if it is enriched in Ba and Cu. For these compositions the critical current density (J _c) at 77 K has an average value of 2×10⁵ A cm^–2, with a tendency for decreasingJ _c with increasing film thickness (0.2 to 0.8m). Variations inJ _c are not correlated with deviations from ideal stoichiometry. Steeper slopes of the resistance-temperature curves above 100 K and lower values of the room-temperature resistivity are associated with high values ofJ _c. If the film composition is enriched in Y relative to Ba and Cu,T _c decreases by several degrees.     

Degradation of thin films of YBa2Cu3O7 by annealing in air and in vacuum

The degradation of epitaxial thin films of YBa₂Cu₃O₇ has been studied as a function of annealing temperature in air and in vacuum; some samples had an evaporated overlayer of CaF₂. Degradation was monitored by the measurement of electrical properties after consecutive 30-min annealing treatments. The room-temperature resistance registered significant increases for all samples after annealing at temperatures above about 200°C; the critical current density at 77 K was degraded for annealing temperatures 400°C in air, and 200–250°C in vacuum. By annealing in oxygen at 550°C, electrical properties were restored in degraded bare YBCO samples annealed in vacuum, but not for those annealed in air.     

Surface resistance of large-area Tl2Ba2CaCu2O8 thin films at microwave and millimeter wave frequencies measured by three noncavity techniques

The surface resistanceR _s of Tl₂Ba₂CaCu₂O₈ films fabricated on LaAlO₃ wafers up to 3 inches (7.6 cm) in diameter through a post-deposition anneal process was measured over the frequency range 5.55–94.1 GHz by the following techniques: 5.55 and 27.5 GHz high-temperature superconductor (HTS)-sapphire resonators, 10 GHz parallel plate resonator, and 94.1 GHz scanning confocal resonator.R _s was found to exhibit a quadratic dependence on frequencyf at 77 K:R _s f ^2.0±0.1. The highest-quality films yieldR _s =145±15 at 10 GHz and 77 K. Scanning confocal resonator mapping ofR _s across a 2-inch (5.1 cm) diameter wafer yielded a base value forR _s of 16±1 m at 77 K and 94.1 GHz (equivalent to 180±10 at 10 GHz) and good uniformity inR _s across the wafer. HTS-sapphire resonator measurements ofR _s for fifteen 1.2 cm square parts cut from a 3-inch diameter wafer yieldedR _s values scaled to 10 GHz of 196±10 at 80 K. Similar values were measured for Tl₂Ba₂CaCu₂O₈ films prepared on both sides of a 2-inch diameter wafer.Rs values at 10 GHz and 80 K of 147–214 were maintained over the course of 40 independent and successive deposition runs and corresponding anneals under nominally identical film fabrication conditions. Surface resistance at 5.55 GHz remained below 80 for maximum rf magnetic fields up to 85 Oe at 4.2 K and 7 Oe at 80 K, respectively. Results are compared with predictions of the two-fluid model. The relative advantages and disadvantages of the different techniques for measuring surface resistance are discussed.     

Microwave properties of highly oriented YBa2Cu3O7-δ superconducting thin films

We have performed millimeter-wave frequency (94 GHz) measurements on high-quality YBa₂Cu₃O₇- superconducting films on yttrium-stabilized (100) ZrO₂ and MgO substrates. The 0.2m thin films fabricated by magnetron sputteringin situ with the YBa₂Cu₃O₇- powders as target exhibit superconducting transition temperatures up to 88 K. The critical current density of 6×10⁵ A/cm² at 77 K and the X-ray diffraction spectrum as well as scanning electron microscope photographs indicate these thin films are fullyc-axis oriented, extremely high in density, and universally homogeneous. Millimeter-wave surface resistances have been measured on a hemisphere open resonator in the temperature range of 20 K toT _c and beyond. The surface resistance at 94 GHz and 77 K for these films is found to be about 30 m, nearly 1/4 that for copper, and a drop of two orders in the surface resistance within 4 K is observed, which indicates that these films are good materials for applications in the millimeter-wave range, especially for fabricating microwave devices. We observed such low surface resistance in these thin films due to the near absence of grain and phase boundaries coupled with a high degree of crystalline orientation.     

Superconducting behavior of high-Tc YBa2Cu3O7 thin films with BaO impurity produced by pulsed laser deposition

We have investigated the superconducting behavior of high-T _c YBa₂Cu₃O₇ (YBCO) thin films containing BaO impure phase produced by pulsed laser deposition. The thin films were characterized by the standard four-probe method, X-ray diffraction (XRD), and scanning electron microscopy (SEM). XRD showed that all these thin films contained BaO impurity, with thec-axis normal to the surface of the substrates. The presence of impurity existed from substrate temperatureT _s of 727 to 796°C. When these thin films with BaO impurity were measured under the magnetic fields, it was found that the critical current densityJ _c increased slightly with increase in magnetic fieldB within the range ofB500 G, in the case ofB perpendicular to thec-axis of the film.     

Fabrication and Transport Properties of MgB2 Thin Films and Tunnel Junctions

We report on fabrication and characterization of MgB₂ thin films and tunnel junction structures. The MgB₂ films were prepared on Al₂O₃, Si, glass, and plastic foil substrates by either vacuum codeposition of boron and magnesium, or high-temperature magnesium annealing of boron films. The crystalline structure of our films depended directly on the method of preparation. The films prepared by codeposition and postannealed in Ar atmosphere were amorphous with nanocrystal inclusions and were characterized by very smooth surfaces. On the other hand, the boron-precursor films annealed in magnesium vapor were rough, polycrystalline with approximately 1-m-diameter single-crystal blocks. Because of their surface quality, the amorphous films were used for preparation of point contact junctions and for optical characterization. The point-contact spectra of tested junctions exhibited a two-gap structure. The MgB₂ polycrystalline films was used for bulk transport studies. The best films were characterized by the critical temperature T _c of up to 39 K and the current density j _c at 4.2 K of about 10⁷ A/cm².     

Large-Area YBa2Cu3O7 ? x Films on Sapphire with Excellent Microwave Power Handling Capability

Crack-free thick YBa₂Cu₃O_{7 – x} films are prepared on CeO₂ buffered r-cut sapphire (2 inch in diameter) with thickness up to 700 nm, smooth surfaces (peak-to-valley roughness <10 nm), high critical currents (J _C > 2 MA/cm² at 77 K and 0 T), and low microwave surface resistances (R _s(77K) .4m and R _s(4.2K) .110 at 19.15GHz) comparable to the best values reported in the literature for YBCO films on structurally better matched substrates. These thick YBCO films were able to handle high microwave power corresponding to magnetic field amplitudes (B _HF) up to 54, 37, and 17.4 mT at 4.2, 50, and 77 K, respectively, which for the lower temperatures were limited by the available power of the 25-W HF amplifier. The high-power performance, which to our knowledge belongs to the best reported so far for unpatterned YBa₂Cu₃O_{7 – x} films, was achieved without any degradation of the samples despite frequent thermal cycling.     

High-Quality YBa2Cu3O7?x Films with CeO2/YSZ Buffer Layers on 2-Inch Si Wafers Deposited by Pulsed Laser

The pulsed laser deposition (PLD) process is shown for in situ reproducibly fabricating YBa₂Cu₃O_7–x (YBCO) superconducting films with yttrium-stabilized zirconia (YSZ) and CeO₂ buffer layers, nonsuperconducting crystalline YBa₂Cu₃O_7–x (YBCO*) passivation layer, and silver contact film on 2-inch silicon wafers. Variations of less than ±7% in film thickness have been obtained for this multilayer growth over the whole wafer. The YBCO films on 2-inch silicon wafers have homogeneous superconducting properties with zero resistance temperature T _c0 from 88.4 K to 88.9 K. and critical current density J _c at 77 K and zero field from 2.5 × 10⁶ to 7× 10⁶ A/cm². The YSZ, CeO₂ and YBCO layers grow epitaxially on silicon wafers. Full widths at half maximum (FWHMs) of (113) reflections of 40 nm thick YBCO layer from -scan patterns are only 1.71° and 1.85° corresponding to the center and edge of the wafer, respectively. These results are very promising for developing high-quality high-T _c superconducting devices on large-area silicon wafers.     

Tl2Ba2CaCu2O8 thin films on 2 in. LaAlO3(0 0 1) substrates

High quality Tl₂Ba₂CaCu₂O₈ (Tl-2212) superconducting thin films are prepared on both sides of 2 in. LaAlO₃(0 0 1) substrates by off-axis magnetron sputtering and post-annealing process. XRD measurements show that these films possess pure Tl-2212 phase with C-axis perpendicular to the substrate surface. The thickness unhomogeneity of the whole film on the 2 in. wafer is less than 5%. The superconducting transition temperatures T_cs of the films are around 105 K. At zero applied magnetic field, the critical current densities J_cs of the films on both sides of the wafer were measured to be above 2 × 10⁶ A/cm² at 77 K. The microwave surface resistance R_s of film was as low as 350 μΩ at 10 GHz and 77 K. In order to test the suitability of Tl-2212 thin films for passive microwave devices, 3-pole bandpass filters have been fabricated from double-sided Tl-2212 films on LaAlO₃ substrates.     

Observation of weakly adsorbed oxygen on Y5Ba6Cu11Oy

We observed, for the first time, adsorption of weakly bonded oxygen at low temperature (<-250°C) by a Y₅Ba₆Cu₁₁O _y sample, using thermogravimetric analysis. The resulting oxygen enriched phase in the surface layers may be attributed to the observation of a superconductivity-like transition at above 200 K.     

Processing of Y1Ba2Cu3Ox Films by Solution Techniques Using Metal-Organic Decomposition

Processing of YBCO films by decomposition of metal trifluoroacetate precursors and its application to the development of coated conductors is investigated. The technique involves preparation of the solution, deposition, and a two-stage heat treatment. A stoichiometric mixture of the acetates of Y, Ba, and Cu and trifluoroacetic acid are used as the starting materials. The glassy residue of the trifluoroacetates of Y, Ba, and Cu formed by drying the above mixture is redispersed in a fixed amount of methanol to provide the starting solution of a given concentration. This solution is then deposited on the substrate surface by the spin coating technique and heat treated in two stages. X-Ray characterization shows that the transformation to 123 is complete in less than 1 h. Pole figure analysis of films deposited on (100) SrTiO₃ and LaAlO₃ single crystal substrates show that these films have a very high degreee of alignment with the substrate both out-of-plane (<0.5°) and in-plane (<1.5°). These chemically derived films were also found to have critical current densities well above 5 × 10⁵ at 77 K for 0.5 m thick films. The applicability of this technique to the production of thick films of YBCO for the development of coated conductors will be discussed.     

Comparative Study of Dense Bulk MgB2 Materials Prepared by Different Methods

We report on the results of a comparative investigation of highly dense bulk MgB₂ samples prepared by three methods: (i) hot deformation; (ii) high pressure sintering; and (iii) mechanical alloying of Mg and B powders with subsequent hot compaction. All types of samples were studied by AC susceptibility, DC magnetization, and resistivity measurements in magnetic fields up to ₀ H = 160 kOe. A small but distinct anisotropy of the upper critical field connected with some texture of MgB₂ grains was found for the hot deformed samples. The samples prepared by high pressure sintering as well as by mechanical alloying show improved superconducting properties, including high upper critical fields H _c2 (₀ H _c2 (0) 23 T), irreversibility fields H _irr which are strongly shifted towards higher values H _irr(T) 0.8 H _c2(T) and high critical current J _c (J _c = 10⁵ A/cm² at 20 K and 1 T).     

The Influence of Bi Doping on the In Situ Growth of TlBa2Ca2Cu3O9 High-Tc Films

The in situ process—laser ablation in combination with thermal evaporation of Tl₂O—has turned out to be a preparation method for single-phase and epitaxial TlBa₂Ca₂Cu₃O₉ (1223) thin films with T _c values up to 109 K. It was found by several groups that a partial substitution of Tl by Bi simplifies the phase development of the 1223 compound in the usual two-step process. We have investigated the influence of the Bi doping on the in situ growth. X-ray measurements show that the films consisted mainly of the 1223 compound. In 300-nm thin films there was no evidence of a Bi amount in the crystal structure, but thinner films (80 nm) show a small amount of Bi. We concluded that Bi doping supports the phase development of the 1223 compound only in an early stage of the film growth. The Bi-doped films have higher T _c values up to 114 K, higher j _c values up to 6 × 10⁵ A/cm² (77 K, 0 T), and lower surface resistances of 56 m (77 K, 87 GHz) than the undoped films.     

Thermoelectric power measurements of YBa2Cu3O7?δ up to 950°C and their application to test the band structure near EF

Four-probe resistivity () and thermoelectric power (TEP) measurements were carried out on samples of YBa₂Cu₃O_7– up to 950°C, in air and in flowing oxygen at 1 bar. Below 700 K the TEP is small and increases rapidly above it, reaching, at 1200 K, +140V/K in air and +120V/K in oxygen. At the changeover temperature (700 K) the slope of log vs.T changes abruptly. These results are interpreted in terms of a model of transport of carriers in a narrow band, which is full for = 1 and half-filled for = 0. Possible origins for such a narrow band are discussed in detail.     

In situ grown superconducting YBCO films on buffered silicon substrates for device applications

Thin films of YBa₂Cu₃O_7– (YBCO) have been grownin situ on silicon single-crystal (100) substrate by using SrTiO₃ as a buffer layer. The deposition has been carried out by on-axis rf magnetron sputtering method. The deposition condition have been optimized by studying the plasma characteristics and correlating them with the superconducting performance of the film. Films deposited at substrate temperature in the range of 680–700°C from stoichiometric YBCO targets in an argon + oxygen mixture (31) are superconducting and showc-axis epitaxy. Compositional confirmation has been carried out using Rutherford backscattering. Scanning tunneling microscopy of the films reveal formation of well-defined layered structure with some defects in the initial stages ofin situ growth of the films. Films grown on SrTiO₃ substrates have excellent crystalline quality (XRD), transition temperatureT _c0=81 K and the critical current densityJ _c >2×10⁵ A/cm² for unpatterned films at 77 K. On silicon substrates using buffer layers thein situ deposited YBCO films shows a higher transition width andT _c0 is also slightly less (71 K).     

Anisotropy in ac losses near the irreversibility field of Bi2Sr2CaCu2O8

The ac susceptibility under a biased dc field near the irreversibility field (H _irr) of a Bi₂Sr₂CaCu₂O₈ single crystal has been measured. The frequency dependence, the ac-power dependence, and the nearly lossless character of the vs.H _dc curve forHa-axis have been roughly explained from a reversible (elastic) fluxoid motion, while those forH c-axis have been explained from a thermally assisted flux-flow (TAFF) model. The obtained parameters are discussed in relation to anisotropic flux-pinning mechanisms in the layered structure of this compound.     

Anisotropy in the resistive superconducting transition under magnetic fields in single crystal Pb2Sr2Ho0.5Ca0.5Cu3O8

Anisotropie properties of the single crystal Pb₂Sr₂Ho_0.5Ca_0.5Cu₃O₈ have been investigated by measuring the electrical resistivity in theab-plane _ab (H, ,T), which depends on the angle between theab-plane and the magnetic-field direction, in various constant fieldsH perpendicular to the current direction. All the angle-dependent values of _ab (H, ,T) at a constant temperature are scaled to be on one curve as a function of reduced field. The anisotropic parameter (m _c ^* /m _ab ^* )^1/2 is estimated as 12–13, which is larger than that of YBa₂Cu₃O₇ and much smaller than that of Bi₂Sr₂CaCu₂O₈. It has been concluded that the anisotropy does not always depend on the thickness of the blocking layer but seems to depend on the overlap of the electronic wave functions along thec-axis. Anisotropy in the pinning potential has also been discussed from the resistive tail in the temperature dependence of _ab (H,,T).     

Electrical properties of non c-axis oriented SrBi2(Ta0.95V0.05)2O9 thin films

Pulsed laser deposition technique was used to grow off c-axis oriented SrBi₂(Ta_0.95V_0.05)₂O₉ (SBTV) ferroelectric thin films. X-ray diffraction studies revealed the c-axis suppression in the films grown at lower substrate temperature (350°C) followed by annealing at higher temperatures (650°C). In-plane lattice parameters of the films were decreased with increase in annealing temperature. SBTV films annealed at 750°C exhibited enhanced ferroelectric properties with remanent polarization (2P _r) of 31.5 C/cm² and coercive field (E _c) of 157 kV/cm. The dielectric permmitivity of the films increased with increase in annealing temperature and it was attributed to the grain size dependence. The films annealed at 750°C showed maximum value of dielectric permittivity 172 with a tangential loss of 0.1, at 100 kHz. Higher value of dissipation factor at lower annealing temperature is explained in terms of space charge accumulation at grain boundaries. The leakage current densities of the films follow ohmic behavior at low field regime and space charge limited current dominates at higher fields.