Fabrication, microstructure and critical current density of screen-printed Ag-(Bi, Pb)2Sr2Ca2Cu3Ox superconducting tapes

The influence of the sintering conditions on the microstructure and critical current density J_c has been studied on screen-printed Ag-(Bi, Pb)₂Sr₂Ca₂Cu₃O_x tapes with a ceramics mono-layer core. Three kinds of fabrication processes, which consist of a combination of cold working (rolling and/or pressing) and sintering, are applied. Four times repetition of pressing and sintering after the pre-sintering produces the highest c-axis alignment and achieves J_c= 1.5 × 10⁴ A/cm² (77 K, 0 T). The J_c versus θ data with an angle θ between B and the c-axis elucidate the relation between the anisotropy ratio γ=J_c(Bc)/J_c(B|c and the half-height angular width Δθ of a peak for Bc. This is related to both grain alignment and the J_c value. An increase in J_c, which comes from an improvement for grain alignment, enhances γ and narrows Δθ. The J_c versus θ data are fitted to the expression J_c(B, θ)=J _c(B, 90°)/[(γ−1)|cos θ|ⁿ+1] by regarding both γ and n as adjustable parameters. Fabrication of screen-printed tapes with multilayers (1≤N≤5) is presented, where the critical current increases from 8.0 A to 30.2 A at 77 K and 0 T as N increases.     

Superconducting properties of ZnO-doped (Bi, Pb)-2223 thick film on Ni and NiO substrates prepared by spray deposition technique

The superconductivity of ZnO-doped (Bi, Pb)-2223 thick film on the Ni and NiO substrates, which was prepared by the spray deposition technique with cold forging, was investigated by characterizing the critical current density (J_c), the critical temperature (T_c), the orientation factor (f), and the microstructure of the film. The thickness of the thick film prepared by the spray deposition method was approximately 10 μm. The maximum J_c value of (Bi, Pb)-2223 film on NiO substrate was approximately 2200 A/cm² (I_c = 110 mA) when the film was sintered at 865 °C for 1 h with a cooling rate of 0.5 °C/min from 865 °C to 650 °C; in the case of Ni substrate, a maximum J_c value of approximately 2000 A/cm² (I_c = 100 mA) was obtained for the (Bi, Pb)-2223 thick film when a cooling rate was 3 °C/min. Such a difference in the J_c values of (Bi, Pb)-2223 thick film on Ni and NiO substrates is attributed to the presence of reaction layer at the (Bi, Pb)-2223 and substrate interface. In addition, the variations in the orientation factor of (Bi, Pb)-2223 thick film on NiO substrate related to those of J_c values. The J_c values of (Bi, Pb)-2223 film on NiO substrate with ZnO doping extremely depended on the amount of ZnO doping and the 0.5 wt% ZnO-doped (Bi, Pb)-2223 thick film deposited on NiO substrate, which was sintered at 835 °C for 1 h in air with a cooling rate of 1 °C/min, showed a J_c value of approximately 1200 A/cm² (I_c = 60 mA). Thus, it is considered that a small amount of ZnO doping was effective in lowering the sintering temperature of (Bi, Pb)-2223 thick film, resulting the improvement in the intragranular weak bonding or Josephson junction.     

Laser ablated bismuth cuprate thin films preparation and effect of oxygen nonstoichiometry upon superconductivity

Thin films of Bi₂Sr₂CaCu₂O₈ and (Bi, Pb)₂Sr₂Ca₂Cu₃O₁₀ have been prepared on monocrystalline (100) MgO substrates, using a laser ablation method with post annealing treatment. The influence of substrate temperature and oxygen pressure during deposition were investigated. SEM observations, EDS analysis, electric and magnetic measurements have been used to characterize the films. Superconducting “2212” films, with T_c(R = 0) at 80–83 K and J_c (50 K) up to 5 × 10⁵ A/cm², have been currently achieved, while Pb-doped “2223” films exhibit T_c as high as 110 K with J_c = 5 × 10⁴ A/cm² at 77 K. The effect of annealing at low temperature (350°C) in an argon flow has been studied for the 2212 phase, it shows the influence of the oxygen non-stoichiometry, i.e. of the hole carrier density upon T_c's which can be measured up to 89 K (zero resistance).     

Influences of Cu composition and sintering condition in Bi-2223 tapes using Ag---Cu alloy sheath doped with Ti, Zr or Hf

Bi-2223 Ag---Cu alloy sheathed tapes doped with Ti, Zr or Hf were fabricated by a powder-in-tube technique using intermediate uniaxial presses and variations in total sintering times. Increasing Cu compositions in the Ag---Cu alloy sheath doped with certain elements into the sheath, combined with appropriate total sintering times were found to lead good superconducting properties. Furthermore, the best total sintering time varied according to the amount of Cu in the Ag---Cu alloy sheath and the existence of doping elements. A transport critical current density, J_c, of 4.1 × 10⁴ A/cm² at 4.2 K, 14 T and 2.2 × 10⁴ A/cm² at 77 K, 0 T was achieved in Ag-10 at% Cu-0.1 at% Hf sheathed Bi-2223 tapes sintered for total 200 h.     

Microstructures in Tl-1223/Ag tapes with different chemical compositions and Jc's

The microstructures of a Tl_0.8Pb_0.2Bi_0.2Sr_1.6Ba_0.4Ca₂Cu₃O_9+δ/Ag tape (tape I) with J_c of 17,600 A/cm² at 77 K and 0 T and three Tl_0.8Pb_0.2Bi_0.2Sr_1.8Ba_0.2Ca_2.2Cu₃O_9+δ/Ag tapes with J_c's of 9300 (tape II), 16,700 (tape III) and 25 200 A/cm² (tape IV) prepared using the powder-in-tube method and an in-situ reaction method, were investigated using high-resolution transmission electron microscopy. In the tape preparation, an intermediate rolling process was incorporated during final heat-treatment for the last tape, but not for the rest of the tapes. Tl-1223 grains are in a thin plate-like shape. Tendency of directional grain-alignment increased in an order of tapes I, II, II and IV. In tape IV, Tl-1223 grains are clearly textured at least partly. In lattice defects, while stacking faults were prevalent in the former composition, dislocations and holes were frequently observed in the latter. Also impurity phases were appeared to be more abundant in the former than in the latter. The relationship between J_c and the microstructure in the tapes was explained in a term of grain-linking.     

High critical current density YBa2Cu3O7−δ tapes prepared by the surface-oxidation epitaxy method

YBa₂Cu₃O_7−δ (YBCO) films with high critical current density (J_c) were successfully fabricated on nickel tapes buffered with epitaxial NiO. NiO was prepared on the textured nickel tape by the surface-oxidation epitaxy (SOE) method. We have reported so far a critical temperature (T_c) of 87 K and J_c=4–6×10⁴ A/cm² (77 K, 0 T) for the YBCO films on NiO/Ni tapes. To enhance the superconducting properties of the YBCO films on the SOE-grown NiO, depositions of thin oxide cap layers such as YSZ, CeO₂, and MgO on NiO were investigated. These oxide cap layers were epitaxially grown on NiO and provided the template for the epitaxial growth of YBCO films. Substantially improved data of T_c=88 K and J_c=3×10⁵ A/cm² (77 K, 0 T) and 1×10⁴ A/cm² (77 K, Hc, 4 T) were obtained for YBCO film on NiO, by using a MgO cap layer with a thickness of 50 nm. The method described in this paper is a simple way to produce long YBCO tape conductors with high-J_c values.     

Performance at 10–50 K of Bi-2212/Ag multilayer tape fabricated by using pre-annealing and intermediate rolling process

High-transport critical current density (J_c-oxide)>500 kA/cm² at 4.2 K, 10 T can be obtained for Bi-2212/Ag tapes fabricated by using pre-annealing and intermediate rolling (PAIR) and melt-solidification process. In this paper, we report high-temperature properties of PAIR-processed Bi-2212/Ag multilayer tape in order to show their potential for practical applications operated at cryocooling temperatures. Magnetic field dependence and angular dependence of critical current (I_c) are investigated at temperatures ranging 10–50 K by using helium gas cooling and liquid neon. Field-temperature curves for I_c=0.2 and 2.0 A are also determined in order to show the approximation of the irreversible field. High-temperature performance of the tape is attractive to consider future applications. For example, the best sample carries I_c=267 A (engineering-J_c=303 A/mm², J_c-oxide=151 kA/cm²) and 92 A (104 A/mm², 52 kA/cm²) at 27.1 K (in liquid neon), in magnetic fields (parallel to the tape surface) of 2 and 10 T, respectively. Engineering-J_c of 100 A/mm² is obtained even in the perpendicular field of 0.5 T at 27.1 K.     

Bi-2223 bar current leads fabricated by the combination of cold isostatic pressing and hot-pressing

A new method using a combination of cold isostatic pressing (CIP) and hot-pressing (HP) was applied to fabricate Bi-2223 bar current leads. The critical current density (J_c) achieved by this method reached as high as 1000 A/cm² at 77 K and self-generated magnetic field. This value of J_c presented here is much higher than the best J_c reported for rod current leads which is 570 A/cm² achieved by CIP technique [Y. Yamada, Bi-based bulk current leads and their applications, in: H. Meada, K. Togano (Eds.), Bismuth-based High-temperature Superconductors, 1996, p. 277.]. The phases and microstructures were analysed by XRD and SEM. The texture and weak link were studied by pole figures and AC susceptibility, respectively. The results show that the grain connectivity, matrix density and texture of the samples were improved significantly by this method.     

Estimation of Jc(B) dependence from self-field alternating current (AC) losses measured on Bi-2223/Ag tapes

Transport AC losses measured in self-field conditions on multifilamentary Bi-2223 tapes are often found to be lower than those calculated within the framework of the critical state model for a bulk wire with elliptical cross section, though generally higher than predicted for a strip. This effect is sometimes ascribed to the non-ideal geometry of the tapes, which does not exactly reproduce either shape. Here we propose an alternative explanation assuming that the critical current density of superconducting material depends on magnetic field. In practice, we analyzed the AC loss curve and deduced different I_c values for the individual data points, using the standard Norris equation for elliptical conductor. This gives the relation between ‘calculated' I_c and the self-field associated to AC transport current, which can be regarded as an alternative way to qualify the dependence of J_c on magnetic field. Important is that this procedure covers the range of fields below the self-field at I_c where the measurement in background DC field can not be used to determine J_c(B).     

Calculation of the critical currents of Bi(2223)/Ag tapes and coils with reduced anisotropy in Ic(B) characteristic — effect of different proportional representations of the filaments oriented parallel and perpendicularly to the tape surface

A mathematical model was developed to allow for the prediction of critical currents in Bi(2223)/Ag-sheathed tapes that consist of two groups of filaments, having crystalline texture (c-axis) predominantly in two directions orthogonal to each other and to the length of the conductor (filaments oriented parallel and perpendicular to the tape surface). Using the theory presented, it is possible to estimate the upper limit of critical currents in the tapes prepared with a two-axial rolling technique. Magnetic field and angular dependencies of critical currents were obtained at 77 K measuring tapes with various proportional representations of filaments oriented in both preferred directions, i.e., the parallel and perpendicular directions. The results of calculation indicate that the anisotropy in the I_c(B) characteristic should be reduced considerably using the two-axial rolling. Unfortunately, the effect of anisotropy reduction is accompanied by simultaneous decrease in the current-carrying capacity of the tapes. The data obtained for short tape samples were utilised to estimate the critical currents of the individual turns of a small cylindrical magnet, assembled of eight pancake coils. It is shown that only a slight increase in the critical current of the magnet can be expected if the winding should be made of the tape with reduced anisotropy in the I_c(B) characteristic. The factors that limit the increase of the magnet critical current are discussed in detail.     

Magnetic and transport properties of YBa2Cu3Oy superconductor foams

The recently reported superconducting YBa₂Cu₃O_y (Y123) foams are highly interesting and promising for variety of applications. In this report we present first magneto-transport measurements of the superconducting properties of these foams. The investigations reveal the superconducting properties being similar to those of bulk melt processed materials. The 123 foams reveal a T_c of 92 K and have a magnetization J_c of 40,000 A/cm² at 77 K and 0 T. The measurements of magnetic hysteresis versus field show a high anisotropy of the critical current density up to J_c^ab/J_c^c7.     

Induction of superconductivity in pulsed laser ablated La2CuO4 thin films by post-deposition fluorination

Pulsed laser ablation has been used to fabricate La₂CuO₄ thin films. Superconducting properties have been successfully induced in the films by an ex-situ, post-ablation annealing process in F₂ gas resulting in a T_c (onset) of 36 K. The presence of two slightly different c-axis expanded phases in the X-ray diffraction data of the fluorinated films implies a degree of inhomogeneity in F₂ uptake. Critical current densities (J_c) and the irreversibility line have been established from hysteresis cycles. A J_c of 10⁶ A cm⁻² for a typical film was observed at 10 K in zero field.     

MgB2超导膜的厚度与其Jc(5K,0T)的关系

通过混合物理化学气相沉积法 (hybrid physical-chemical vapor deposition, HPCVD), 在(000l) SiC 衬底上制得一系列从10 nm到8 μm的MgB₂超导膜样品, 并对它们的形貌、超导转变温度T_c 和临界电流密度J_c与膜厚度的关系进行了研究. 观察到T_c随膜厚度增加上升到最大值后, 尽管膜继续增厚, 但T_c值保持近乎平稳, 而J_c则先随膜厚度增加上升到最高值后, 继而则随膜的厚度的增加而下降. MgB₂膜的T_c(0)和T_c(onset)值与膜厚的关系基本一致, T_c(0)在膜厚为230 nm处达到最大值T_c(0)=41.4 K, 而J_c(5K,0T)在膜厚为100 nm时达到最大值, J_c (5 K, 0 T)=2.3×10⁸A·cm^-2, 这也说明了我们能用HPCVD方法制备出高质量干净MgB₂超导膜. 本文研究的超导膜厚度变化跨度非常大, 从10 nm级的超薄膜到100 nm级的薄膜, 再到几微米的厚膜, 如此T_c和J_c对膜厚度变化的依赖就有了较完整、成体系的研究. 并且本文的工作对MgB₂超导薄膜制备的厚度选取具有实际应用意义. 关键词： 2超导膜')" href="#">MgB₂超导膜 混合物理化学气相沉积法 厚度 临界电流密度     

Synthesis of YBa2Cu3O7−x superconducting thin films on LaAlO3 by means of PAMOCVD

High-T_c superconducting thin films have been deposited in situ by means of a plasma assisted metal-organic chemical vapour deposition (PAMOCVD) process on LaAlO₃. An EMCORE high-speed rotating disc reactor was used to deposit the films at a substrate temperature of 600°C to 800°C. The system is equipped with a (remote) 120 W microwave plasma generator. The oxidising plasma gas is N₂O and/or O₂ while Ar was used as the inert carrier gas for the different metal-organics. The influence of different process parameters (such as the temperatures of the metal-organics, substrate temperature, and plasma gas composition) on the superconductive properties and on the morphology of the films was investigated. Surface morphology and composition were studied by SEM/EDX or EPMA, and AC susceptibility measurements were used to investigate the superconductive properties (T_c and J_c). X-ray diffraction measurements indicated that single-phase YBa₂Cu₃O_7−x films were epitaxially grown with the 00l orientation perpendicular to the substrate surface. The critical temperature (T_c) of the films is about 90 K and the critical current density (J_c) is higher than 10⁶ A/cm² at 77 K and zero field.     

Effect of unidirectional solidification rate on Jc for current lead

The dependence of transport J_c value on the traveling rate and the nominal composition was investigated by taking different nominal compositions of YBa₂Cu₃O_6+x (Y123) + n mol% Y₂BaCuO₅ (Y211) (n = 10, 20, 30, 40 and 50) with addition of 0.5 wt% of Pt on samples processed by different unidirectional solidification rates, namely 1, 3 and 5 mm/h. The highest J_c was found in the sample with 30% Y211 addition by the higher traveling rate adjusted to prevent the formation of polycrystals. In this φ 1.56 × 60 mm sample the values of transport I_c and J_c were 1370 A and 71 700 A/cm², respectively, which were obtained by the conventional DC four-probe method with criterion of 1 μV/cm at 77 K and self-field.     

Granularity, microstructure, and flux creep in TlBa2Ca2Cu3O9+δ superconducting powder and silver-sheated tapes

Silver-sheathed TlBa₂Ca₂Cu₃O_9+δ (Tl-1223) tapes, with a transport critical current density, J_ct, of 6200 A/cm² at 75 K under zero magnetic field, were fabricated by the oxide-powder-in-tube (OPIT) method and characterized using an X-ray diffractometer (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), and superconducting quantum interference device (SQUID) magnetometer. The results of the magnetization and SEM study indicate that, in these tapes, individual grains are distributed randomly in orientation and weak links exist. However, strongly linked percolative current paths within the tape persisting in increasing fields, accompanied by strong intrinsic interplanar coupling, sustain a significant J_ct at high fields and lead to the plateau in the J_ct-H curve. Dislocation networks, which may act as effective pinning centers, are the common features observed in the tapes. To investigate the effects on flux pinning due to thermomechanical processing, magnetic relaxation at 1 and 2 T over 5–50 K was measured. The tape shows slightly lower normalized relaxation rates (S=-(1/M_o)dM/ dln t) than the cauliflower-like precursor powder. Analyses of the relaxation data obtained from the tape, after incorporating temperature dependence and field scaling, yield an expression for the effective pinning energy U_eff(J,T,H) = (U₁/H^0.54)[1-(T/ 72.5)²]⁴(J/J_i)^μ. This result was compared with the prediction of the collective flux-creep model, which suggests that Tl-1223 has a three-dimension-like (3D-like) vortex lattice. Presumably, a more plate-like powder morphology may result in improved texturing by the OPIT process. Tl_0.5Bi_0.5Sr₂CaCu₂O_7+δ ((Tl,Bi)-1212) powder with this morphology was therefore synthesized for comparison.     

Phase evolution during the melting and recrystallization of ceramic core in the (Bi,Pb)-2223 tape

The phase evolution during melting and recrystallization of (Bi,Pb)₂Sr₂Ca₂Cu₃O₁₀ ((Bi,Pb)-2223) core in a Ag-sheathed monofilamentary tape has been investigated. The tape was fabricated by PIT process with powders containing nearly pure (Bi,Pb)-2223 phase. Short samples were melted at 805 °C, 808 °C, 812 °C, 816 °C, 831 °C, slowly cooled at 1.5 °C/h under flowing 1.6% O₂ balanced with argon and quenched in air at room temperature. X-ray diffraction (XRD) and scanning electron microscopy coupled with energy dispersive spectroscopy (SEM/EDS) were applied for the phase identification. The results show that (Bi,Pb)-2223 core is partially melted into a liquid and alkaline earth cuprates (AECs), mainly 2:1-AEC, at 805 °C, 808 °C, 812 °C, and well reforms directly from the melt during the slow cooling. More (Bi,Pb)-2223 phase is decomposed at temperatures higher than 816 °C, but cannot recrystallize, indicating that a partial melting at some temperatures around a given temperature range is essential to (Bi,Pb)-2223 phase reformation. The melt composition moves from that between “2223” and “2212” stoichiometries towards 2212-like stoichiometry with increasing temperature. This seems to lead to the conclusion that (Bi,Pb)-2223 phase decomposes incongruently into a 2212-like liquid and (Ca,Sr)-cuprates. 2:1-AEC plays the most important role in (Bi,Pb)-2223 melt-recrystallization process. Our results also reveal that plate-like shape (Bi,Pb)-2223 grains can be obtained via melting and recrystallization if the optimum processing conditions are used.     

Critical current density of polycrystalline YBa2Cu3O7−δ consisting of tin-coated grains

Tin and its oxides have been introduced into the intergrain areas of polycrystalline YBa₂Cu₃O_7−δ by coating the crystalline grains with a thin layer of tin and sintering the ceramics in flowing oxygen and argon. The transport critical current density J_c at 77 K in a magnetic field of 0−1.5 T is enhanced as a result of the coating. A probable improvement of the intergrain weak links is suggested.     

Reduced filament coupling in Bi(2223)/BaZrO3/Ag composite tapes

Multifilamentary Bi(2223)/Ag tapes often exhibit AC loss levels comparable to those measured in monofilamentary samples, which is partly due to the large coupling currents induced in the low resistive sheath material. Surrounding the individual filaments by electrically insulating barrier layers suppresses these currents and strongly reduces the coupling. We demonstrate this effect with various types of magnetic and self-field AC loss measurements on a series of Bi(2223)/BaZrO₃/Ag tapes. We also discuss the influence of barrier thickness, twist pitch length and filament arrangement on the measured losses in these composite conductors.     

Thermal transport in the oxygenated magnetic superconductor, Eu1.5Ce0.5RuSr2Cu2O10+δ

The thermal conductivity and thermopower are reported for a hole doped Eu_1.5Ce_0.5RuSr₂Cu₂O_10+δ sample that has been annealed at 1100 K under an oxygen pressure of 54 atm. At T_c=45 K superconductivity and weak ferromagnetism coexist (T_m=180 K). Weak features in the thermopower, S(T), and thermal conductivity, κ(T), are observed both at T_m and at T^*=140 K. The thermopower begins to decrease sharply toward zero at T_c, and there is an extremely sharp increase of about 30% in the thermal conductivity at T_c. This “first order” transition may be related to the sudden appearance of a spontaneous vortex phase at T_c. A small shoulder is observed in κ(T) in the temperature range T=5–13 K.