Effect of processing temperature on the superconducting properties of acetone doped MgB2 tapes

Correlation of phase formation, critical transition temperature T_c, microstructure, and critical current density J_c with sintering temperature has been studied for acetone doped MgB₂/Fe tapes. Sintering was performed at 600–850 °C for 1 h in a flowing Ar atmosphere. High boron substitution by carbon was obtained with increasing the sintering temperature; however, the acetone doped samples synthesized at 800 °C contain large size MgB₂ grains and more MgO impurities. Incomplete reaction for the acetone doped samples heated at 600 °C result in bad intergrain connectivity. At 4.2 K, the best J_c value was achieved in the acetone doped sample sintered at 700 °C, which reached 24,000 A/cm² at 10 T and 10,000 A/cm² at 12 T, respectively. Our results indicate that the small grain size and less impurity were also important for the improvement of J_c–B properties besides the substitutions of B by C.     

Synthesis and characterization of excess magnesium MgB2 superconductor under inert carbon environment

The structural, transport and magnetic properties of MgB₂ superconductor heavily blended with Mg is studied. The samples are synthesized with a new approach in both, pressed carbon environment and in flowing argon. The excess magnesium used is observed to play dual role: one being the prevention of Mg losses during the synthesis process and hence maintaining the stoichiometry of MgB₂ phase, and second being the formation of Mg milieu probably all around the MgB₂ grains to give a dense structure. Excess Mg also improves the grain connectivity by going into the pores and there by minimizing the insulating junctions. The residual resistivity of the sample is observed to decrease from 57.02 μΩ cm to 10.042 μΩ cm as it is progressively filled with superconductor–normal–superconductor (SNS) type junctions amongst the grains by the virtue of increased magnesium content. The synthesized samples devoid of porosity show the superconducting transition, T_c in the range of 39–34 K as of clean MgB₂ samples, though overloaded with Mg. The excess Mg resulted in enhanced critical current density, J_c from 6.8 × 10³ A cm^?2 to 5.9 × 10⁴ A cm^?2 at 20 K and 10 kOe, with reasonable decrease in the superconducting transition. Thus our samples being overloaded with Mg impart mechanical strength and competitive superconducting properties, which forms a part of interest.     

Effect of W-addition on pinning property of MgB2

The 5d transition metal W was added into the MgB₂ superconductor. The Mg, B and W were sintered at 1173 K for 30 min under H₂/Ar atmosphere in the electric furnace. The W_x(MgB₂)_1?x samples were prepared in the W concentration range of 0 ? x ? 0.05. Temperature and field dependences of magnetization were measured by the SQUID magneto-meter. The field and x dependences of J_c at 20 K were analyzed by the extended critical state model. The enhancement of J_c became maximum for the x = 0.02 sample.     

Pinning,thermally activated depinning and their importance for tuning the nanoprecipitate size and density in high Jc YBa2Cu3O7−x films

YBa₂Cu₃O_7?x (Y123) films with quantitatively controlled artificial nanoprecipitate pinning centers were grown by pulsed laser deposition (PLD) and characterized by transport over wide temperature (T) and magnetic field (H) ranges and by transmission electron microscopy (TEM). The critical current density J_c was found to be determined by the interplay of strong vortex pinning and thermally activated depinning (TAD), which together produced a non-monotonic dependence of J_c on c-axis pin spacing d_c. At low T and H, J_c increased with decreasing d_c, reaching the very high J_c ～ 48 MA/cm² ～20% of the depairing current density J_d at 10 K, self-field and d_c ～ 10 nm, but at higher T and H when TAD effects become significant, J_c was optimized at larger d_c because longer vortex segments confined between nanoprecipitates are less prone to thermal fluctuations. We conclude that precipitates should extend at least several coherence lengths along vortices in order to produce irreversibility fields H_irr(77 K) greater than 7 T and maximum bulk pinning forces F_p,max(77 K) greater than 7–8 GN/m³ (values appropriate for H parallel to the c-axis). Our results show that there is no universal pin array that optimizes J_c at all T and H.     

Intrinsic pinning properties of FeSe0.5Te0.5

The intrinsic pinning properties of FeSe_0.5Te_0.5, which is a superconductor with a critical temperature T_c of approximately 14 K, were studied through the analysis of magnetization curves obtained using an extended critical state model. For the magnetization measurements carried out with a superconducting quantum interference device (SQUID), external magnetic fields were applied parallel and perpendicular to the c-axis of the sample. The critical current density J_c under the perpendicular magnetic field of 1 T was estimated using the Kimishima model to be equal to approximately 1.6 × 10⁴, 8.8 × 10³, 4.1 × 10³, and 1.5 × 10³ A/cm² at 5, 7, 9, and 11 K, respectively. Furthermore, the temperature dependence of J_c was fitted to the exponential law of J_c(0) × exp(?αT/T_c) up to 9 K and the power law of J_c(0) × (1 ? T/T_c)ⁿ near T_c.     

Flux pinning in columnar-structured and single crystalline MgB2 films

We have investigated the flux pinning effect of columnar grain boundary in columnar-structured and single crystalline MgB₂ films. The MgB₂ films with columnar structure showed much higher J_c than that of single crystalline thin film, and sample having smaller grain size had a higher J_c in high magnetic fields. At 5 K, the MgB₂ film with grain size of 460 nm showed an abnormal double-peak behavior in pining force density, F_p(B), caused by competition of different types of pinning sites, such as planar defects and point defects. Field dependences of F_p in columnar-structured films suggest that the columnar grain boundary is a strong pinning source in the MgB₂ film and it plays a crucial role in enhancing J_c over a wide range of magnetic fields and temperatures.     

Stoichiometry dependence of the critical current density in pure and nano-SiC doped MgB2/Fe tapes

The stoichiometry dependence of the microstructure and superconducting properties of pure and nano-SiC doped MgB₂/Fe tapes was systematically investigated. The tapes prepared with the composition of a slight deficiency of Mg (Mg_0.9B₂ and Mg_xB₂(SiC)_0.1 (x = 0.9 and 1.0)) showed the best transport J_c. Adding a slight excess of Mg like 5%, as being done by many researchers, was not beneficial for the J_c improvement as expected. The onset T_c was not significantly changed in both doped and undoped tapes by adding excess of boron or magnesium, but the transition widths were broadened due to the induced impurities. The slightly-Mg-deficient pure samples show smaller grain sizes, which corresponds to a better J_c–B performance at high magnetic field due to the enhanced grain boundary pinning. The field dependence of J_c in nano-SiC doped tapes was almost not influenced by varying the starting Mg content although microstructural difference can still be seen, suggesting that the flux pinning ability was mainly controlled by the carbon substitution effect for boron.     

Strongly enhanced flux pining of GdBCO coated conductors with BaSnO3 nanorods by pulsed laser deposition

We report the effects of BSO addition on the crystallinity, texture, and the field dependency of critical current density (J_c) of GdBCO coated conductors (CCs) prepared by pulsed laser deposition (PLD). Undoped and BSO-doped GdBCO films showed only c-axis oriented growth, and the incorporated BSO nanorods exhibited epitaxial relationship with the GdBCO matrix. In comparison with undoped film, BSO-doped GdBCO film exhibited greatly enhanced J_c and higher pinning force densities in the entire field region of 0–5 T (H//c) at 77 and 65 K. The BSO-doped GdBCO film showed the maximum pinning force densities (F_p) of 6.5 GN/m³ (77 K, H//c) and 32.5 GN/m³ (65 K, H//c), ～2.8 times higher than those of the undoped sample. Cross-sectional TEM analyses exhibited nano-structured BSO nanorods roughly aligned along the c-axis of the GdBCO film, which are believed effective flux pinning centers responsible for strongly improved critical current densities in magnetic fields.     

Thickness dependence of Ic and Jc of LTG-SmBCO coated-conductor on IBAD-MgO tapes

We have reported SmBa₂Cu₃O_y (SmBCO) films on single crystalline substrates prepared by low-temperature growth (LTG) technique. The LTG-SmBCO films showed high critical current densities in magnetic fields compared with conventional SmBCO films prepared by pulsed laser deposition (PLD) method. In this study, to enhance critical current (I_c) in magnetic field, we fabricated thick LTG-SmBCO films on metal substrates with ion-beam assisted deposition (IBAD)-MgO buffer and estimated the I_c and J_c in magnetic fields.All the SmBCO films showed c-axis orientation and cube-on-cube in-plane texture. T_c of the LTG-SmBCO films were 93.1–93.4 K. J_c and I_c of a 0.5 μm-thick SmBCO film were 3.0 MA/cm² and 150 A/cm-width at 77 K in self-field, respectively. Those of a 2.0 μm-thick film were 1.6 MA/cm² and 284 A/cm-width respectively. Although I_c increased with the film thickness increasing up to 2 μm, the I_c tended to be saturated in 300 A/cm-width. From a cross sectional TEM image of the SmBCO film, we recognized a-axis oriented grains and 45° grains and Cu–O precipitates. Because these undesired grains form dead layers, I_c saturated above a certain thickness. We achieved that I_c in magnetic fields of the LTG-SmBCO films with a thickness of 2.0 μm were 88 A/cm-width at 1 T and 28 A/cm-width at 3 T.     

Effects of doping with nanoscale Co3O4 particles on the superconducting properties of powder-in-tube processed MgB2 tapes

Nanoscale Co₃O₄ particles were doped into MgB₂ tapes with the aim of developing superconducting wires with high-current-carrying capacity. Fe-sheathed MgB₂ tapes with a mono-core were prepared using the in situ powder-in-tube (PIT) process with the addition of 0.2–1.0 mol% Co₃O₄. The critical temperature decreased monotonically with an increasing amount of doped Co₃O₄ particles for all heat-treatment temperatures from 600 to 900 °C. However, the transport critical current density (J_c) at 4.2 K varied with the heat-treatment temperatures. The J_c values in magnetic fields ranging from 7 to 12 T decreased monotonically with increasing Co₃O₄ doping level for a heat-treatment temperature of 600 °C. In contrast, some improvements on the J_c values of the Co₃O₄ doped tapes were observed in the magnetic fields below 10 T for 700 and 800 °C. Furthermore, J_c values in all the fields measured increased as the Co₃O₄ doping level increase from 0 to 1 mol% for 900 °C. This heat-treatment temperature dependence of the J_c values could be explained in terms of the heat-treatment temperature dependence of the irreversibility field with Co₃O₄ doping.     

Influence of Zr and Ce doping on electromagnetic properties of (Gd,Y)–Ba–Cu–O superconducting tapes fabricated by metal organic chemical vapor deposition

(Gd,Y)Ba₂Cu₃O_x tapes have been fabricated by metal organic chemical vapor deposition (MOCVD) with Zr-doping levels of 0–15 mol.% and Ce doping levels of 0–10 mol.% in 0.4 μm thick films. The critical current density (J_c) of Zr-doped samples at 77 K, 1 T applied in the orientation of H 6 c is found to increase with Zr content and shows a maximum at 7.5% Zr doping. The 7.5% Zr-doped sample exhibits a critical current density (J_c) of 0.95 MA/cm² at H 6 c which is more than 70% higher than the J_c of the undoped sample. The peak in J_c at H 6 c is 83% of that at H 6 a–b in the 7.5% Zr-doped sample which is more than twice as that in the undoped sample. Superconducting transition temperature (T_c) values as high as about 89 K have been achieved in samples even with 15% Zr and 10% Ce. Ce-doped samples with and without Ba compensation are found to exhibit substantially different J_c values as well as angular dependence characteristics.     

Effects on Jc of pinning center morphology for multiple-in-line-damage in coated conductor and bulk,melt-textured HTS

The properties of discontinuous aligned pinning centers (PCs) created by high-energy heavy-ions are compared for bulk melt-textured and coated conductor HTS. Properties of PCs, which increase J_c (pinning potential and entanglement), and negative properties which decrease J_c (e.g., decreased T_c and percolation paths) are evaluated. Mechanisms are proposed to explain the very large increases in J_c resulting from multiple-in-line-damage (MILD) compared to continuous columnar pinning centers (CCPC). In particular, a mechanism which results in fluxoid entanglement, even for parallel (unsplayed) PCs, is discussed. The same mechanism is found to also account for restoration of much of the pinning potential expected to be lost due to the gaps in MILD PCs. It also accounts for the fact that at high fluence, J_c increases as fluence is increased, instead of decreasing as expected. The very low self-field in coated conductor permits separation of the negative and positive effects of PCs. It is found that parameters developed to quantify the negative effects in bulk melt-textured YBCO, by 63 GeV U²³⁸ ions, successfully describe damage to 2.1 μm thick coated conductor by 1 GeV Ru⁴⁴ ions. Coated conductor at 77 K and self-field is generally known to have J_c about 100 times that of melt-textured YBCO. However, at 77 K and applied field of 1 T, when both forms of HTS are processed with comparable numbers of near-optimum MILD PCs, the difference in J_c is reduced to a factor of 1.3–2. Whereas J_c for melt-textured YBCO increased sharply, by a factor of up to 16.8 for high-fluence MILD PCs, J_c in coated conductor increased by a smaller factor of 2.5–3.0. Nevertheless, 2.1 μm thick coated conductor, with near-optimum MILD PCs, exhibits J_c = 543 kA/cm² at 77 K and applied field of 1.0 T, and I_c = 114 A/cm-width of conductor. This is the highest value we find in the literature. The phenomenology developed indicates that for optimum MILD PCs in coated conductor, J_c ～ 700 ± 70 kA/cm² should be achievable at 77 K, 1.0 T.     

Effects of nanoscale defects on critical current density of (Y1−xEux)Ba2Cu3O7−δ thin films

In pulsed laser deposition of YBa₂Cu₃O_7?δ films, defect introduction into the films tends to anisotropically improve the pinning along the H||c direction due to the columnar growth mode of the process. In Eu-substituted samples, however, even though an increase in critical current density (J_c) in the H||c direction was observed for low fields (H = 0.2 T), the improvement was more notable for the H||ab-plane at both low and higher fields. Herein we present detailed TEM microstructural studies to understand these new trends in J_c(H), which are markedly different than flux pinning increases achieved with other methods, for example, with nanoparticle additions. Threading dislocations, observed in the Eu-substituted samples along the c-axis, account for J_c enhancement with H||c at low field. The enhanced ab-planar pinning in the Eu-substituted samples is attributed to the extensive bending of the {0 0 1} lattice planes throughout the film, and the crystal lattice defects with excess Cu–O planes, that were effective in increasing the J_c for H||ab at both low and high fields.     

Large transport critical currents of powder-in-tube Sr0.6K0.4Fe2As2/Ag superconducting wires and tapes

We report the achievement of transport critical currents in Sr_0.6K_0.4Fe₂As₂ wires and tapes with a T_c = 34 K. The wires and tapes were fabricated through an in situ powder-in-tube process. Silver was used as a chemical addition as well as a sheath material. All the wire and tape samples have shown the ability to transport superconducting current. Critical current density J_c was enhanced upon silver addition, and at 4.2 K, a largest J_c of ～1200 A/cm² (I_c = 9 A) was achieved for 20% silver added tapes, which is the highest in iron-based wires and tapes so far. The J_c is almost field independent between 1 T and 10 T, exhibiting a strong vortex pinning. Such a high transport critical current density is attributed to the weak reaction between the silver sheath and the superconducting core, as well as an improved connectivity between grains. We also identify a weak-link behavior from the apparent drop of J_c at low fields and a hysteretic phenomenon. Finally, we found that compared to Fe, Ta and Nb tubes, Ag was the best sheath material for the fabrication of high-performance 122 type pnictide wires and tapes.     

Effect of ball milling time on the substitution of carbon in glucose doped MgB2 superconductors: Dispersion behavior of glucose

The effect of the ball milling time (BMT) on the substitution of the carbon in the glucose doped MgB₂ samples is investigated here. Using in situ solid state reaction, four different doped samples of Mg(B_.98C_.02)₂ were prepared by mixing powders of Mg, boron and glucose for 2 h, 4 h, 8 h and 12 h using planetary ball milling. A reference sample of un-doped MgB₂ was also prepared under same conditions. The particle size distribution of the un-reacted samples show a decrease in the particle size as the BMT is increased. Both the average particle size as well as the standard deviation show a substantial decrease with the increase in the milling time up to 8 h. After 8 h, the size reduction is rather insignificant. From the XRD data, the crystallite size of the doped MgB₂ computed using the Scherrer formula was found to decrease with the increasing BMT, showing a saturation level after 8 h of the milling time. TEM images also confirm the crystallite size obtained from the XRD data. The substitution of the C in the MgB₂ lattice, measured from the change in the c/a ratio, increases with increasing BMT. The maximum carbon substitution is achieved at approximately 8 h of BMT. Moreover, a systematic enhancement of the residual resistivity and a decrease in T_C with an increasing BMT further confirms a progressive substitution of the carbon in the MgB₂. These results suggest that a minimum ball milling time is necessary to disperse the glucose uniformly for a maximum substitution of nano C in the B plane of MgB₂ lattice. The optimum BMT is found to be 8 h. Thus, the decrease in the particle size due to the ball milling enhances the dispersion of the constituent materials thereby favoring a greater substitution of the dopant in the MgB₂ during the solid-state reaction.     

Increase of critical current density with doping carbon nano-tubes in YBa2Cu3O7−δ

The effects of carbon nano-tubes (CNTs) on the crystal structure and superconducting properties of YBa₂Cu₃O_7?δ (Y-123) compound were studied. Samples were synthesized using standard solid-state reaction technique by adding CNT up to 1 wt% and X-ray diffraction data confirm the single phase orthorhombic structure for all the samples. Current–voltage measurements in magnetic fields up to 9 T were used to study the pinning energy U_J and critical current density J_c as a function of magnetic field at fixed temperature. We find that while T_c does not change much with the CNT doping (91–92 K), both U_J and J_c increase systematically up to 0.7 wt% CNT doping in a broad magnetic field ranges between 0.1 and 9 T and J_c in the 0.7 wt% CNT doped sample is at least 10 times larger than that of the pure Y-123. The scanning electron microscope image shows that CNTs are forming an electrical-network between grains. These observations suggest that the CNT addition to the Y-123-compounds improve the electrical connection between superconducting grains to result in the J_c increase.     

Fabrication of Ti doped MgB2/Cu superconducting wires by SHS method in an unsealed furnace

Mg_0.9Ti_0.1B₂/Cu wires have been successfully synthesized by the powder-in-tube (PIT) technique combined with the self-propagating high-temperature synthesis (SHS) method in an unsealed furnace. The analysis includes the studies of the sample microstructure, phase composition, critical transition temperature T_c and critical current density J_c. The experiments show that the PIT technique combined with the SHS method is effective in reducing the Mg volatilization and oxidation. There is little reaction between Mg and Cu in the SHS process, but with the MgCu₂ and CuO phases, the reaction does occur in the inner sheath wall of the copper tube. The findings also indicate that there is little MgO in the sample. The sample has a very strong flux pinning ability at the low magnetic fields since the TiB₂ phase may prevent the growth of MgB₂ grains and lead to a favorable effect on grain refinement. The wires exhibit a high critical current density, e.g. 2.7 × 10⁵ A/cm² in the 1.0 T field at 4.2 K and 1.3 × 10⁵ A/cm² in the 2.0 T field at 4.2 K.     

MgB2 coated superconducting tapes with high critical current densities fabricated by hybrid physical-chemical vapor deposition

The MgB₂ coated superconducting tapes have been fabricated on textured Cu (0 0 1) and polycrystalline Hastelloy tapes using coated conductor technique, which has been developed for the second generation high temperature superconducting wires. The MgB₂/Cu tapes were fabricated over a wide temperature range of 460-520 °C by using hybrid physical-chemical vapor deposition (HPCVD) technique. The tapes exhibited the critical temperatures (T_c) ranging between 36 and 38 K with superconducting transition width (ΔT_c) of about 0.3-0.6 K. The highest critical current density (J_c) of 1.34 × 10⁵ A/cm² at 5 K under 3 T is obtained for the MgB₂/Cu tape grown at 460 °C. To further improve the flux pinning property of MgB₂ tapes, SiC is coated as an impurity layer on the Cu tape. In contrast to pure MgB₂/Cu tapes, the MgB₂ on SiC-coated Cu tapes exhibited opposite trend in the dependence of J_c with growth temperature. The improved flux pinning by the additional defects created by SiC-impurity layer along with the MgB₂ grain boundaries lead to strong improvement in J_c for the MgB₂/SiC/Cu tapes. The MgB₂/Hastelloy superconducting tapes fabricated at a temperature of 520 °C showed the critical temperatures ranging between 38.5 and 39.6 K. We obtained much higher J_c values over the wide field range for MgB₂/Hastelloy tapes than the previously reported data on other metallic substrates, such as Cu, SS, and Nb. The J_c values of J_c(20 K, 0 T) ∼5.8 × 10⁶ A/cm² and J_c(20 K, 1.5 T) ∼2.4 × 10⁵ A/cm² is obtained for the 2-μm-thick MgB₂/Hastelloy tape. This paper will review the merits of coated conductor approach along with the HPCVD technique to fabricate MgB₂ conductors with high T_c and J_c values which are useful for large scale applications.     

Carbon doping of MgB2 by toluene and malic-acid-in-toluene

The decomposition of malic acid (C₄H₆O₅) in the presence of Mg and B was studied using Differential Scanning Calorimetry (DSC) and Thermogravimetric Analysis (TGA) which revealed that malic acid reacted with Mg but not B. Also, the addition of toluene (C₇H₈) to dissolve malic acid followed by subsequent drying resulted in no reaction with Mg, indicating that the malic acid had decomposed during the dissolution/drying stage. The total carbon contributed by toluene versus a toluene/5 wt.% malic acid mixture was measured using a LECO CS600 carbon analyzer. The toluene sample contained ～0.4 wt.% C while the toluene/malic acid mixture had ～1.5 wt.% C, demonstrating that the toluene contributed a significant amount of carbon to the final product. Resistivity measurements on powder-in-tube MgB₂ monofilamentary wires established that the toluene/malic acid doped sample had the highest B_c2. However, the toluene-only sample had the highest transport J_c over most of the magnetic field range (0–9 T), equaled only by that of toluene/malic-acid sample in fields above 9 T.     

Preparation of solution-based YBCO films with BaSnO3 particles

The YBCO films with BaSnO₃ (BSO) particles were prepared on LAO (0 0 1) substrates by metal organic deposition using trifluoroacetates (TFA-MOD) via introducing SnCl₄ powders into the YBCO precursor solution. It was found that with the increase of the SnCl₄ contents, the slower decomposition and higher temperature for nucleation during the reaction were requested compared to that of pure YBCO film. The YBCO films with different contents of Sn with dense surface and well c-alignment were obtained under optimized heat treatment, and the BaSnO₃ phases were detected by XRD analysis. Litter effect of BSO particles on the T_c and J_c values of YBCO films was found. All YBCO films with BSO particles had T_c values over 90 K and J_c values over 1 MA/cm². A significant enhancement of J_c was observed for YBCO films with BSO particles compared to that of pure YBCO film by the field dependence of J_c values. The best property was obtained for YBCO film with 6 mol.% Sn at 77 K under magnetic field. The results showed that the J_c value of YBCO film with 6 mol.% Sn was enhanced by a factor of 2 in 2 T, and over a factor of 10 beyond 4 T compared to that of pure YBCO film.