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Materials Express 2158-5849/2014/4/105/010 Copyright © 2014 by American Scientific Publishers All rights reserved. Printed in the United States of America doi:10.1166/mex.2014.1153 www.aspbs.com/mex Critical current density improvement by intermediate deformation for the fabrication of Bi2Sr2Ca2Cu3O10+/Ag round wires Peng Xie1 , Timing Qu1, 2, ∗ , Kaite Huang1 , Feng Feng1, 3 , and Zhenghe Han1 1 Applied Superconductivity Research Center, Department of Physics, Tsinghua University, Beijing 100084, China Key Laboratory for Advanced Materials Processing Technology, Department of Mechanical Engineering, Tsinghua University, Beijing 100084, China 3 Division of Advanced Manufacturing Graduate School at Shenzhen, Tsinghua University, Shenzhen 518055, China 2 Delivered by Ingenta to: ? Multi-filamentary Bi2 Sr2 Ca2 Cu3 OIP: /Ag round wires were11fabricated the powder-in-tube method. Both drawOn: Fri, Aug 2017by 16:19:37 10+5.10.31.210 Copyright: Scientific ing and cold isostatic pressing methods wereAmerican used to densify thePublishers filament cores of the Bi2 Sr2 Ca2 Cu3 O10+ /Ag round wires during intermediate deformation after the first heat treatment. Critical current measurements show that both methods can increase the self-field critical current density at 77 K. By optimizing the drawing process, the core density of the first heat treated round wires was increased significantly, resulting in a more than doubled critical current density improvement of the Bi2 Sr2 Ca2 Cu3 O10+ /Ag round wires. Increasing the drawing stress using a high strength metal sheath increased the critical current density further to about 1 × 104 A/cm2 . By carrying out the intermediate deformation using the cold isostatic pressing method, the optimal critical current density was 8.6 × 103 A/cm2 . Keywords: Powder in Tube Method, Superconductor, Drawing, Cold Isostatic Pressing, Core Density, Critical Current Density. 1. INTRODUCTION High temperature superconducting (HTS) materials including Bi2 Sr2 Ca2 Cu3 O10+ /Ag (Bi-2223/Ag) wires, Bi2 Sr2 Ca1 Cu2 O8+ /Ag (Bi-2212/Ag) wires and YBa2 Cu3 O7− (YBCO) coated conductors have been widely used in various applications, such as cables, magnets, motors, transformers, fault current limiters, superconducting magnetic energy storages, etc.,1–4 due to their high critical current density (Jc ) and feasible operation at liquid nitrogen temperature. Most of the HTS wires were fabricated into a tape geometry having a large aspect ratio of 15–40. However, there were at least two disadvantages which restricted ∗ Author to whom correspondence should be addressed. Email: [email protected] the application of these HTS tapes. (1) Electro-magnetic anisotropy: usually the Jc of the tape under the perpendicular field was much lower than that under the parallel field,5–7 which arose from the intrinsic flux pinning anisotropy of the cuprate superconductors.8 (2) Mechanical anisotropy: the HTS tapes can only be bent along the tape surface due to both their high aspect ratio and their brittle ceramic core characteristics. Therefore, for many applications, round HTS wires are preferable. Both Bi2212/Ag and MgB2 round wires have been developed for applications operating below 20–30 K.9–13 However, for operating temperatures above 30 K, studies of YBCO or Bi-2223/Ag round wires are few in number.14–16 For Bi2223/Ag tape, it is easy to increase the superconducting core density and enhance the filament texture. However, Mater. Express, Vol. 4, No. 2, 2014 105 Article ABSTRACT Article Materials Express Critical current density improvement for Bi-2223/Ag round wires Xie et al. for round wires, it is much more difficult. In order to keep drawing die, and thus the diameter of the wire was the round geometry, flat rolling or uniaxial pressing proreduced. The wire cross sectional area reduction per drawcesses usually used in tape fabrication are not suitable. ing pass was about 7%, and the die angle was 13.5 . Drawing could only yield an upper limit of core density The drawing was carried out at a speed of 0.5 m/s without (∼ 70% of the theoretical core density) for lacking of large lubrication. stress imposed on the powder.17 Besides, the filament texDrawing with metal sheaths was also carried out. As ture also cannot be significantly improved for lacking of shown in Figure 2, brass sheath of 1.7 mm/0.8 mm flat rolling process.18 These are the reasons for very few (outer diameter of 1.7 mm and inner diameter of 0.8 mm) reports on the Bi-2223/Ag round wires over the years. As and stainless steel sheath of 1.2 mm/0.8 mm were far as we know, the highest Jc of Bi-2223/Ag round wires adopted, respectively. After drawing, the outer sheath of is 3.2 × 104 A/cm2 reported by Fujikami, and consist of a brass or steel was corroded by a 30 wt.% FeCl3 solution concentric arrangement of filaments.16 It has low packing with heating in a water bath at 80 C for about 1 hour. ratio (∼ 12%) of Bi-2223 powder and high ratio of the silThe CIP process was carried out at a pressurization rate ver matrix in the cross section of the wire. As a result, the of 5 MPa/s, and held for 60 seconds upon reaching the Ic of the wire is low too. Xiaodong Su’s work showed that target pressure to obtain the CIP samples. Water was used the intermediate drawing process is supposed to be necesto transmit the pressure during the CIP process. To prevent sary to increase the critical current (Ic ) of round wires.15 permeation of water into the superconducting cores from Recently, the cold isostatic pressing (CIP) method was the two ends of the wire, which can cause a failure of the introduced into the fabrication of Bi-2212/Ag wires and CIP process, the HT1 treated samples were inserted into the critical current density of Bi-2212/Ag wires can be the 0.1 mm thick polyethylene terephthalate (PET) bag, doubled.19 and then the bag was vacuumized and thermoplastically In this work, various methods including drawing, drawsealed to keep the pressure in the bag below 0.1 atm. ing with high strength sheath sleeving and cold isostatic A Nikon ME600 optical microscope was used to pressing were used to increase the core density, hoping to observe cross sections of the deformed round wires. increase the Jc of the round wire. Both the core density and Micrographs and elemental analysis were obtained on a deforthe Jc were increased by optimizing the mechanical Leo-1530 electronic microscope (SEM) equipped Delivered by Ingenta to: scanning ? mation process. Meanwhile, an effective way to enhance with an Oxford energy IP: 5.10.31.210 On: Fri, 11 Aug 2017 16:19:37 dispersive spectroscopy (EDS) sysCopyright: American Scientific Publishers the local 2223 filament texture was explored. tem in the backscattered electron (BSE) imaging mode. Self-field Ic values of fully-processed wires were obtained using the standard four-probe method with a criterion of 2. EXPERIMENTAL DETAILS 1.0 V/cm over the temperature range 77 K to 4.2 K. InThe traditional powder-in-tube (PIT) method was used to field Ic was measured with applied field up to 8 T at 4.2 K fabricate 61 filaments Bi-2223/Ag green round wire havand 0.075 T at 77 K, respectively. The image processing ing a diameter of 0.8 mm. The heat treatment procesoftware-Photoshop was used to calculate the filling facdure is shown in Figure 1. The first heat treatment (HT1) tor, which is defined as the ratio of the core cross sectional was carried out at 830 C for 20 hours in an atmosphere area to the total wire cross sectional area. with a reduced oxygen partial pressure (pO2 = 008 bar). Intermediate mechanical deformation was carried out by 3. RESULTS AND DISCUSSION either the drawing method or the CIP method. Then, the main heat treatment (MHT) was carried out to obtain the 3.1. Intermediate Drawing Process fully-processed round wires by sintering at 830 C with 3.1.1. The Critical Current Performance a subsequent slow-cooling process in an atmosphere with In the fabrication of Bi-2223/Ag tapes, it has been found pO2 = 008 bar. that intermediate mechanical deformation is crucial for During the intermediate drawing process, for each drawobtaining high Jc performance.20 21 Thus, in this work, ing pass, the HT1 treated wire was drawn through a the intermediate drawing process was introduced between the two heat treatments to improve the Jc of the Bi2223/Ag round wires. The drawing samples were obtained by drawing the HT1 treated samples to different diameters. The relation between the Jc values and the diameter of the drawing samples is shown in Figure 3. The original diameter of the green wire was 0.80 mm. The Jc value of the reference sample without intermediate drawing was around 3600 A/cm2 (shown by the solid square point in Fig. 3). As the diameter of drawing samples decreased, the Jc value first increased and then decreased. The Jc Fig. 1. The fabrication procedure of Bi-2223/Ag round wire. reached its maximum value of about 8300 A/cm2 when 106 Mater. Express, Vol. 4, 2014 Critical current density improvement for Bi-2223/Ag round wires Xie et al. Materials Express Fig. 2. The optical photos of the samples: (a) the cross section of the Bi-2223/Ag round wire; (b) the cross section of the Bi-2223/Ag round wire with brass sheath sleeving; (c) the cross section of the Bi-2223/Ag round wire with steel sheath sleeving; (d) the appearance of the three kinds of wires for intermediate deformation. the diameter was around 0.71 mm. Therefore, Jc of round wires was more than doubled by introducing the intermediate drawing process. If the diameter of the drawing sample was reduced further still, the Jc of the wire would Fig. 3. The Jc of the drawing samples (green wire of 0.80 mm) variation with different diameter. The error bars represent the standard deviation of the Jc data. The samples fabricated without intermediate drawing were shown in solid symbol. The samples fabricated with intermediate drawing were shown in hollow symbols. Mater. Express, Vol. 4, 2014 decline. The similar result was found in Bi-2223/Ag tapes by Grasso.22 who pointed out that large deformation led to the formation of cracks in the superconducting cores and thus suppressed Jc . For the drawing sample having a diameter of 0.71 mm, the relation between the Ic (self field) and the temperature is shown in Figure 4(a). The Ic of the Bi-2223/Ag round wire was 15 A at 77 K, and it became larger as the temperature decreased. When the sample was cooled to 4.2 K, Ic reached 80 A. The Ic increased by a factor of 5 as the temperature decreased from 77 K to 4.2 K, which was similar to Bi-2223/Ag tape results.23 The in-field Ic results are shown in Figure 4(b). Ic decreased rapidly as the applied field increased when the applied field was below 0.1 T at 77 K. Even at 4.2 K, Ic reduced significantly until the applied field reached 1 T. The total Ic of the Bi-2223 tape can be seen as the sum of the weak link critical current-Icw and the strong link critical current-Ics . At 77 K, Icw decreases fast even before 101 –102 mT, while the Ics retains until several tesla. The transport capacity of the weak-link can be easily reduced by the increasing external field. Therefore, the fast decrease of Ic below 0.1 T at 77 K and 1 T at 4.2 K indicated that large amount 107 Article Delivered by Ingenta to: ? IP: 5.10.31.210 On: Fri, 11 Aug 2017 16:19:37 Copyright: American Scientific Publishers Article Materials Express Critical current density improvement for Bi-2223/Ag round wires Xie et al. The details of the drawing sample having an optimum diameter— 0.71 mm can be observed in Figures 5(d) and (e). Many outgrowth Bi-2223 grains are observed to have grown into the silver matrix, as shown in Figure 5(d), and some adjacent filaments are connected by these outgrowth grains. A similar phenomenon in Bi-2212/Ag wires has been investigated by Shen,24 who pointed out that the growth of Bi-2212 grains between filaments can form filament to filament bridging composed of two types of bridges: one having a potential high-Jc path and the other not. We considered that the outgrowths observed in our work led to bridging similar to the latter one, which did not carry much current. As shown in Figure 5(d), at the inner part of the filaments, many thin Bi-2223 grains formed with random orientation, which were not well textured and connected. Between these randomly oriented Bi-2223 grains, some several m-sized CuO or SrO grains can be observed. These non superconducting phases and the residual voids in the filaments can block the current flow and cause a Jc decrease. The weak-link existed due to the low core density and the irregular alignment of Bi-2223 grains compared to the microstructure of Bi-2223/Ag tapes, which contributed to the fast decrease of Ic in low fields, as shown in Figure 4(b). In each filament, however, along the Delivered by Ingenta to: ? superconducting-silver IP: 5.10.31.210 On: Fri, 11 Aug 2017 16:19:37 interface, a Bi-2223 layer with a thicknessPublishers of 2–4 m formed with good texture, as shown Copyright: American Scientific in Figure 5(e), which can provide good supercurrent paths. Moreover, it is interesting to point out that, as the intermediate drawing proceeded, many Bi-2223 layers along the superconducting-silver interfaces intersected to form acute angles at the corners of the filaments, as shown in Figures 5(c) and (d). In these local regions, the two Fig. 4. (a) Self-field Ic of 0.71 mm Bi-2223/Ag round wire (optimized drawing sample), as the temperature changing from 77 K to adjacent Bi-2223 layers in the filament could grow com4.2 K. (b) In-field Ic of Bi-2223/Ag round wire (being 0.71 mm with pactly to form a 10 m thick Bi-2223 region, as shown filling factor of 43.5%) at 4.2 K and 77 K. in Figure 5(f), and the angle between the two adjacent Bi-2223 layers was small at these corners. Because the Jc through the grain boundaries is very sensitive to the orienof weak-link existed in the present round wire. The intation of adjacent crystallites and increases exponentially field Ic can be further improved if the weak links could be with decreasing misorientation angle,25 these acute correduced. ners of the filaments with large Bi-2223 grains and small angle grain boundaries could be potential high-Jc supercur3.1.2. The Micro Structure Evolution rent paths. As discussed above, the Jc of the Bi-2223/Ag SEM micrographs of fully-processed drawing samples round wires could be further improved by increasing the having a diameter in the range 0.80 mm to 0.71 mm are superconducting-silver interfaces and the local acute angle shown in Figure 5. A number of voids can be observed in regions of the superconducting filaments. Figure 5(a) for the sample fabricated without intermediate drawing. For the samples fabricated with intermediate 3.1.3. The Core Density Variation drawing, shown in Figures 5(b) and (c), the voids were As the diameter of round wires decreased during the drawlargely reduced as the diameter of the drawing samples ing process, the filling factor–rsc first decreased and then decreased. Meanwhile, the filament shapes changed, and stopped decreasing and stabilized with some fluctuation, a number of silver-superconducting interfaces intersected as shown in Figure 6. Any given section of Bi-2223/Ag to form acute angles at the corners of the filaments as the wire is a composite of two parts: one is the superconductdiameter decreased, which will be discussed later in this subsection. ing filament array and the other is the silver matrix, as 108 Mater. Express, Vol. 4, 2014 Critical current density improvement for Bi-2223/Ag round wires Xie et al. Materials Express Article Delivered by Ingenta to: ? IP: 5.10.31.210 On: Fri, 11 Aug 2017 16:19:37 Copyright: American Scientific Publishers Fig. 5. The SEM micrographs of the cross section of the fully-processed drawing samples. (a) The sample of 0.80 mm fabricated without intermediate drawing; (b) the sample fabricated with intermediate drawing to 0.75 mm; (c) the sample fabricated with optimum intermediate drawing to 0.71 mm; (d) the detail of several filaments (sample of 0.71 mm); (e) the Bi-2223 texture along the superconducting-sliver interface; (f) the Bi-2223 phase at the corners of the filaments. shown in Figure 2(a). During the fabrication process, the following relations are always satisfied: Ag Sr Ag l = MAg sc Sr sc l = Msc (1) where Ag and sc are the mass densities of the silver matrix and superconducting cores, respectively. MAg and Msc are the mass of the silver matrix and superconducting cores, respectively, rAg is the ratio of the silver matrix to the total round wire cross sectional area, rsc is the ratio of the superconducting cores to the total round wire cross sectional area, where these two ratios satisfy rAg + rsc = 100%. S is the total cross sectional area and l is the length of the wire. By solving Eq. (1), we obtain: sc = k · 1 − rsc rsc where the coefficient k is given by: k = Ag · Msc /MAg Mater. Express, Vol. 4, 2014 (2) During the fabrication process, the silver matrix mass and the superconducting core mass are constants, and also the density of silver matrix is almost unchanged. Therefore, the coefficient k is a constant. As shown in Eq. (2), the core density–sc depends only on the filling factor—rsc . For green round wires with no heat treatment, we calculated the filling factor when drawing the wire. The rsc value stabilized at 50% when the diameter of the green wire was from 1.2 mm to 0.8 mm. However, as indicated in Figure 6, for the drawing samples which had already been sintered for 20 hours at HT1, the rsc reduced from 50% to 43% after the intermediate drawing process. Therefore, from Eq. (2) the core density sc increased by 32.5% after the intermediate drawing process. This could be explained by that: during the green wire drawing process, if the drawing parameters were fixed, there existed an upper limit for the core density.17 26 However, during sintering, the voids formed throughout the aggregate, as shown in Figure 5(a). Drawing after sintering could 109 Materials Express Article Fig. 6. The rsc variation with the diameter of drawing samples. The sample fabricated without intermediate drawing was shown in solid symbol. The samples fabricated with intermediate drawing were shown in hollow symbols. The dash line was assisted to observation. Critical current density improvement for Bi-2223/Ag round wires Xie et al. Fig. 7. The relation between the Je and the diameter of Bi-2223/Ag wires. The error bars represent the standard deviation of the Je data. “”: Intermediate drawing with no sleeving for comparison; “”: Intermediate drawing with brass sheath sleeving; “”: Intermediate drawing with steel sheath sleeving. As a comparison, the samples fabricated without intermediate drawing were shown in solid symbols. The samples fabricated with intermediate drawing were shown in hollow symbols. further decrease these voids and therefore increase the core density. As shown in Figure 6, the relationship between rsc and the diameter in the drawing process can be divided into two regions: (1) the rsc decreases when drawing the wire metal sheaths were corroded to make oxygen diffusion from 0.80 mm to 0.71 mm, corresponding to an possible in the subsequent heat treatment. increase in the core density; (2) the rsc remains stable when The relationship between the engineering critical curDelivered to: ? the diameter is below 0.71 mm, corresponding to a coreby Ingenta rent density e ) and the diameter of fully-processed brass Aug 2017(J16:19:37 density saturation, i.e., about 63.0%IP: of 5.10.31.210 the theoreticalOn: den-Fri, 11 or steel sleeved samples is shown in Figure 7. The Je Copyright: Publishers sity by the estimation in our experiment. SimilarAmerican results Scientific of the brass sleeved samples and steel sleeved samples were found in the Bi-2223/Ag tape study conducted by both increased with decreasing diameter. However, the Han et al.17 They proposed a “powder-flow” model to Je of the brass sleeved samples were no better than the explain such results. Powder flow will stop when the fricordinary drawing samples without sleeving. Whereas, for tion between powder grains is equal to the driving force on steel sleeved samples, the Je could be improved to 4.02 × the powder, thus the powder packing density reaches a crit103 A/cm2 , and the rsc was about 40.7%. Because Jc = ical value. Further density increase requires an increase of Je /rsc , the maximum Jc value reached 9.88 × 103 A/cm2 . the drawing stress by modifying the drawing parameters. As far as we know, this is a Jc record for 61 filaments As indicated in Figures 3 and 6, both the Jc and the Bi-2223/Ag round wires, although it is lower than the Jc core density of the round wire increased as the diameter (3.2 × 104 A/cm2 ) of the round wire composed of condecreased, which demonstrates again that the Jc is related centrically arranged filaments reported by Fujikami.16 to the core density.27 To increase the Jc further, the superWe speculate that the higher Jc value reported for wire conducting core should be further densified to form more with concentrically arranged filaments is owing to betcompact Bi-2223 grains. ter texture relative to our samples. As we mentioned in 3.1.4. Drawing with High Strength Metal Sheaths During the intermediate drawing process, a compressive stress was imposed on the Bi-2223 powder via the silver matrix which contains an outer silver alloy sheath and inner pure silver filament walls. Considering that the silver matrix is ductile and its yield strength is not high enough, the stress imposed on the powder was limited. As a result, the possible increase of the core density was limited. In this work, drawing with high strength metal sheaths was used to further densify the core. Brass and stainless steel sheaths were used to sleeve the HT1 treated round wire, respectively. Then the sleeved Bi-2223/Ag wires were drawn by different passes, and finally, the sleeved 110 Section 3.1.2, the grain alignment of our wire could be improved by carrying out the intermediate deformation. The final goals of improving Bi-2223 texture in the present work and in the literature (16) are consistent. Improving the texture of the round wire further should be our next target. Nevertheless, the multifilament Bi-2223/Ag round wires shown in this work are more easily produced on an industrial scale, and it have a larger packing ratio, which means the amount of silver can be greatly reduced for the present round wires. During the drawing process, the maximum stress applied on the powder is limited by the strength of the outer sheath. In previous studies, using Ag alloys rather than pure Ag may have made it possible to apply a Mater. Express, Vol. 4, 2014 Critical current density improvement for Bi-2223/Ag round wires Xie et al. Materials Express authors.33 34 By carrying out CIP at different stages of tape fabrication, the core density has been raised and the critical current density also enlarged. However, as far as Yield Tensile we know, fabrication of Bi-2223/Ag round wire using Material strength (MPa) strength (MPa) intermediate CIP processing has not yet been reported. Pure silver 6529 17030 In this work, the CIP process on samples of HT1 treated 31 Silver alloy (AgMg01 Ni01 ) 160–180 230–240 (self test) Bi-2223/Ag round wires was conducted. A sample fabriBrass (UNS C26000) 145 310–420 cated without CIP treatment is shown in Figure 8(a), in Stainless steel (UNS S30400) 240 585 which a number of voids are observed. As the CIP pressure was increased to 200 MPa, the voids were only slightly reduced, as shown in Figure 8(b). However, Figures 8(c) larger drawing stress and therefore increase the final core and (d) indicate that the voids in the filaments were greatly density.17 Therefore, we considered that the cores might reduced for both samples fabricated with a CIP pressure be further densified by drawing with other metal sheaths, of 400 MPa and 590 MPa, respectively. of which the mechanical strengths are stronger than that of The relationship between the diameter of CIP samples silver alloys. Generally, the outer sheath goes through plasand the CIP pressure is shown in Figure 9. The origitic deformation during the drawing process, and the stress nal diameter was 0.805 mm and it slightly reduced to required to sustain plastic deformation of the material is 28 0.803 mm when the pressure was increased to 100 MPa. the flow stress, which is a function of the plastic strain. The wire diameter reduced sharply from 0.803 mm to The flow stress equals the yield strength of the material at 0.758 mm as the pressure increased from 100 MPa to which plastic flow is initiated, and in most cases it rises as 300 MPa. As the CIP pressure continued to increase, the plastic strain increases due to work hardening of the the diameter reduction rate slowed, and finally, the diammaterial. Because the initial stress and the maximum stress eter reduced to 0.746 mm when the pressure reached during plastic deformation are respectively determined by 590 MPa. Although the diameter of the wire could be the yield strength and the tensile strength, the flow stress reduced remarkably as the CIP pressure increased, no elonusually resides in between. gation of the wire was observed after the CIP process (the Delivered Table I lists the yield strength and the tensile strengthby Ingenta to: ? original length was 12 cm). During the CIP process, the IP: in 5.10.31.210 On: Fri, 11 Aug 2017 16:19:37 values of the metal materials used our experiment. wire always satisfies the following conditions: Copyright: American Scientific Publishers The yield strength values of the silver and silver alloy are about 65 MPa and 160 MPa–180 MPa, respectively, SAg + Ssc = d 2 /4 SAg + Ssc = d 2 /4 which determine the minimum stress required to cause where SAg and Ssc are the cross sectional areas of the plastic deformation of the wire. The flow stress genersilver matrix and the superconducting cores of the HT1 ated by the brass sheath during drawing was close to that treated wire, respectively. SAg and Ssc are the cross secof the silver alloy. While the flow stress generated by tional areas of the silver sectional areas of the silver matrix the steel sheath was much larger than that of the silver and the superconducting cores of the CIP treated wire, alloy. As a result, the stress enhancement might be limited respectively. Besides, d and d are the diameters of the by drawing with a brass sheath. However, a much larger HT1 treated wire and the CIP treated wire, respectively. compressive stress could be imposed on the powder by The volume of the silver matrix was assumed to be condrawing with a stainless steel sheath to increase the core stant throughout the CIP process, and there was no elondensity so as to increase the Jc . It should be noted that gation. Consequently, the cross sectional area of silver the optimal Jc of steel sleeved samples was very close to matrix was constant, indicating that SAg = SAg . Thus, we 4 2 1 × 10 A/cm , almost 1/6–1/3 of the Jc of commercial Bican obtain: 2223/Ag tapes. A possible way to further enhance the Jc SAg /Ssc + 1 is drawing with even higher strength sheath materials like = d/d 2 (3) 32 SAg /Ssc + Ssc /Ssc Hastelloy C276, which is commonly used as a substrate for coated conductors. As mentioned in 3.1.3, the rsc of the HT1 treated wire was 50%, and, as a result, SAg /Ssc equaled to 1. By sub3.2. Cold Isostatic Pressing (CIP) stitution into Eq. (3), we obtain: As shown above, core densification by introducing the Ssc d/d 2 intermediate drawing process was crucial for Jc improve= (4) Ssc 2 − d/d 2 ment of Bi-2223/Ag round wires. Another effective way to increase the core density is the CIP method. During As the superconducting core density increase is inversely the CIP process, a controlled uniform pressure is applied proportional to its area reduction if the wire length is fixed, simultaneously to the entire external surface of the sample. thus, we obtain: S Improving of the critical current density of Bi-2223/Ag Nsc = sc = sc (5) tapes by the CIP method has been reported by some sc Ssc Table I. The yield strength (0.2% offset) and tensile strength of the materials used in this study. 111 Article Mater. Express, Vol. 4, 2014 Materials Express Critical current density improvement for Bi-2223/Ag round wires Xie et al. Article Fig. 8. The SEM micrographs of the CIP samples with different CIP pressure. (a) The HT1 treated sample with no CIP treatment; (b) the sample of 200 MPa CIP treatment after HT1; (c) the sample of 400 MPa CIP treatment after HT1; (d) the sample of 590 MPa CIP treatment after HT1. where Nsc is the relative core density normalized to the The Jc value of the HT1 treated wire without intermediate was around 3500 A/cm2 . As the CIP core density of the HT1 treated wire. Combining Eqs. (4) Delivered by Ingentadeformation to: ? pressure increased, Jc increased slowly when the pressure and (5), we deduce: IP: 5.10.31.210 On: Fri, 11 Aug 2017 16:19:37 was below 100 MPa, then it increased rapidly over the Copyright: American Scientific Publishers d/d 2 pressure range of 100 MPa–300 MPa and stabilized at Nsc = (6) 2 − d/d 2 8.6 × 103 A/cm2 in the pressure range 300 MPa–590 MPa. The effect of pressure on the Jc demonstrated in The calculated variation in Nsc with CIP pressure is also Figure 9 was much smaller when the CIP pressure was shown in Figure 9. When the pressure was below 100 MPa, below 100 MPa than when the pressure was between the Nsc was almost unchanged. After that, the Nsc increased 100 MPa and 300 MPa. This can be explained by with increasing CIP pressure and reached its maximum, the fact that the yield strength of the silver alloy a 39.8% density increase compared with the HT1 treated (AgNi01 Mg01 wt.% in this work) was 160–180 MPa.31 cores, when the pressure was 590 MPa. The Jc variation A CIP pressure lower than the yield strength of the outer with the CIP pressure was nearly simultaneous to the Nsc sheath could not produce a plastic deformation of the variation, as shown in Figure 9. sheath. As a result, there was no obvious effect on the core densification, and the improvement of the Jc was not significant. When the CIP pressure was above 200 MPa, which exceeded the yield strength of the silver alloy, an effective plastic deformation of the wire took place, corresponding to the significant wire diameter reduction observed. Thus, the superconducting cores were densified and the Jc of the round wire was rapidly improved. However, the Jc value of the 590 MPa sample was not higher than that of the 300 MPa sample. A possible reason could be a lack of shear stress between grains during the CIP process,17 33 which could limit the Jc improvement. Besides, the maximum CIP pressure in this work was 590 MPa, which is already close to the triple point of water at high pressure and room temperature (liquid, Fig. 9. “”: The Jc of the CIP samples variation with the CIP presice V and ice VI phases coexist in thermodynamic equisure. “”: The diameter of the CIP samples variation with the CIP pressure “”: The normalized core density Nsc variation with the CIP librium at 618.4 MPa and 0.16 C).35 We considered that pressure. The error bars represent the standard deviation of the data. CIP treatment with even larger pressure should increase 112 Mater. Express, Vol. 4, 2014 Critical current density improvement for Bi-2223/Ag round wires Xie et al. Materials Express the core density further. Therefore, another pressure transmitting medium should be used to obtain a CIP pressure above 618.4 MPa. More work on the CIP treatment of Bi-2223/Ag round wires will be carried out in the future. Mater. Express, Vol. 4, 2014 113 Article 6. F. Feng, T. M. Qu, C. Gu, Y. Xin, W. Z. Gong, W. Wu, and Z. Han; Comparative study on the critical current performance of Bi-2223/Ag and YBCO wires in low magnetic fields at liquid nitrogen temperature; Physica C 471, 293 (2011). 7. V. Lombardo, E. Barzi, D. Turrioni, and A. V. Zlobin; Critical currents of YBa2 Cu3 O7− tapes and Bi2 Sr2 CaCu2 Ox wires at different temperatures and magnetic fields; IEEE Trans. Appl. Supercond. 4. CONCLUSION 21, 3247 (2011). In this study, multi-filamentary Bi-2223/Ag round wires 8. J. R. Clem; Anisotropy and two-dimensional behaviour in the were fabricated by the PIT method in conjunction with high-temperature superconductors; Supercond. Sci. Technol. 11, 909 an intermediate deformation process. The Jc value of (1998). the round wire can be more than doubled by optimizing 9. W. T. Nachtrab, C. V. Renaud, J. T. Wong, X. T. Liu, T. M. Shen, the intermediate drawing process. During the intermediU. P. Trociewitz, and J. Schwartz; Development of high superconductor fraction Bi2 Sr2 CaCu2 Ox /Ag wire for MRI; IEEE Trans. Appl. ate drawing process, core densification is believed to be Supercond. 18, 1184 (2008). the primary reason for the Jc improvement of the resulting 10. K. R. Marken, H. P. Miao, M. Meinesz, B. Czabaj, and S. Hong; Bi-2223/Ag round wires. Besides, local acute corners of Progress in Bi-2212 wires for high magnetic field applications; IEEE the filaments formed during intermediate drawing can be Trans. Appl. Supercond. 16, 992 (2006). potential high-Jc current paths owing to the formation of 11. T. Hasegawa, N. Ohtani, T. Koizumi,Y. Aoki, S. Nagaya, N. Hirano, large and compact Bi-2223 grains with small angle grain L. Motowidlo, R. S. Sokolowski, R. M. Scanlan, D. R. Dietderich, boundaries. The flow stress of the outer metal sheath durand S. Hanai; Improvement of superconducting properties of Bi2212 round wire and primary test results of large capacity Rutherford ing deformation can be an important factor for Jc improvecable; IEEE Trans. Appl. Supercond. 11, 3034 (2001). ment. By drawing with a stainless steel sheath, the Jc 12. H. W. Weijers, U. P. Trociewitz, K. Marken, M. Meinesz, H. Miao, can be further increased with an optimal value as high as and J. Schwartz; The generation of 25.05 T using a 5.11 T 9.88 × 103 A/cm2 . By the CIP method, the Jc and the Nsc Bi2 Sr2 CaCu2 Ox superconducting insert magnet; Supercond. Sci. increased simultaneously as the CIP pressure increased, Technol. 17, 636 (2004). 3 2 and the optimal Jc value was 8.60 × 10 A/cm . 13. S. Mine, H. Song, M. Xu, J. Marte, S. Buresh, W. Stautner, C. Immer, E. T. Laskaris, and K. Amm; Test coil for the developto: ? Acknowledgment: This work is supported Delivered by the Pro-by Ingenta ment of a compact 3 T MgB2 Magnet; IEEE Trans. Appl. Supercond. IP: 5.10.31.210 On: Fri, 11 Aug 2017 16:19:37 gram of International S&T Cooperation (2010DFA64510) 22, 4400604 (2012). Copyright: American Scientific Publishers 14. P. Li, L. Zhao, T. M. Qu, X. C. Wang, and Z. Han; Fabrication and and the Fundamental Research Program of Science study of thin Bi-2223 round wires; Physica C 463, 837 (2007). and Technology Development Foundation of Shenzhen 15. X. D. Su, G. Witz, R. Passerini, K. Kwasnitza, and R. Flukiger; (JCYJ20120614193005764, JCYJ20130402145002389). Square and round Bi(2223) wire configurations and their AC losses; We are grateful to Dr. Xuejie Zhang at Chinese Academy Physica C 372, 942 (2002). of Agricultural Sciences (CAAS) for offering the CIP 16. J. Fujikami, K. Hayashi, H. Takei, S. Honjo, T. Mimura, K. Matsuo, equipment and many helpful discussions. We would like and Y. Takahashi; HTS transposed cable conductor and round shape to thank Jiayin Lin for the low temperature measurement strand. 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