Magneto-optical imaging of flux patterns in multifilamentary (BiPb)2Sr2Ca2Cu3Ox composite conductors U. Welp, D. O. Gunter, G. W. Crabtree, J. S. Luo, and V. A. Maroni Materials Science Division, Argonne National Laboratory, Argonne, Illinois 60439 W. L. Carter American Superconductor Corporation, Westborough, Massachusetts 01581 V. K. Vlasko-Vlasov and V. I. Nikitenko Institute for Solid State Physics, 142432 Chernogolovka, Moscow District, Russia ~Received 14 October 1994; accepted for publication 22 December 1994! We present a study of the superconducting morphology of the transport current carrying cross section of a 19-filament ~BiPb!2Ca2Cu3Ox ~Bi-2223! composite conductor using magneto-optical imaging of magnetic flux patterns. In conjunction with electron microscopy on the same sample this technique allows a unique correlation of superconducting and microstructural properties. Direct evidence for enhanced superconducting properties in platelike regions along the silver/Bi-2223 interface and for weak properties near the core of the filaments is obtained. Misaligned grain colonies are found to cause an interruption of the superconducting continuity in the filaments. © 1995 American Institute of Physics. A central goal of research on high-temperature superconducting ceramics is the establishment of a methodology for the reliable fabrication of long length wire for use in magnet systems and ac power transmission technology. At present, the most promising systems are silver-sheathed ~BiPb!2Sr2Ca1Cu2Ox ~Bi-2212! and ~BiPb!2Sr2Ca2Cu3Ox ~Bi-2223! composites. Critical current densities J c at 77 K in self-field in excess of 10 000 A/cm2 have been reported1 for lengths exceeding a kilometer. Further improvement of the performance of these conductors seems possible if the limiting factors in the present materials can be identified. In recent studies it has been shown that the conductor does not respond uniformly across its cross section to an imposed transport current. By slicing a Bi-2223 monofilament composite into strips parallel to the rolling direction Larbalestier et al.2 showed that J c in the center of the filament is strongly reduced as compared to J c near the edges which are in intimate contact with the silver sheath. In a systematic comparison of microstructure and critical current density Merchant et al.3 observed that high performance conductors are characterized by a substantial degree of texturing of the Bi-2223 grains. This texture develops between superconductor and silver sheath during the heat treatment phase of the thermomechanical processing cycle ~reaction induced texture!. A recent transmission electron microscopy ~TEM! study4 on cross sections of monofilamentary Bi-2223 composites confirms the presence of a highly textured almost phase-pure Bi-2223 layer at the Ag/Bi-2223 interface, with second phases more prominent toward the interior of the conductor. Critical current densities of 100 000 A/cm2 in this thin interface layer were observed by Lelovic et al.5 by peeling off the majority of a Bi-2223 monofilament. A recent magnetooptical study on a longitudinal cross section of a Bi-22231 and of a Bi-22126 conductor showed substantial variation of J c along the rolling direction. Here we report the first direct observation of the nonuniformity of the superconducting behavior in the transverse 1270 Appl. Phys. Lett. 66 (10), 6 March 1995 cross section ~i.e., the transport current carrying cross section! of a 19-filament Ag/Bi-2223 composite as function of temperature and applied magnetic field using a highresolution magneto-optical technique. With increasing temperature and especially with increasing field a pronounced superconducting granularity in the filament develops. We present the first direct evidence for the occurrence of highpinning platelets near the Ag/Bi-2223 interface and a region of weaker pinning in the center of the filaments. Also in cross sections presented further on two interconnects between neighboring filaments are observed. Whereas one of them does not carry a supercurrent at high temperatures and fields the other is a strong link at all temperatures and fields studied. The importance of such superconducting interconnects between filaments for the evaluation of ac losses is discussed. A comparison with scanning electron microscopy ~SEM! images of the same cross section allows a close correlation of the observed magnetic flux patterns with the microstructure. The magnetic patterns were recorded using a highresolution magneto-optical technique as described before.7 It is based on the Faraday effect in a yttrium–iron–garnet film placed on top of the sample. The enhanced optical sensitivity allows the observation of flux patterns in fields up to 1000 G at temperatures as high as 77 K with a spatial resolution of about 3 mm. These temperature and field conditions are close to the expected practical operating conditions of high-T c superconducting cables. The Bi-2223 composite conductor studied here was prepared using the oxide-powder-in-tube ~OPIT! process which has been described in detail elsewhere.8 The composite contains 19 filaments that lie in an intermediate packing pattern9 of 3, 4, 5, 4 and 3 filaments edge-to-edge. The critical current of this conductor is 35 A at 77 K in self-field. Details magnetic flux images were taken near an edge pack and near the center pack of the composite. These two areas experienced a large difference in total de- 0003-6951/95/66(10)/1270/3/$6.00 © 1995 American Institute of Physics FIG. 1. SEM image @panel ~a!# and magnetic flux patterns at 30 K @panel ~b!# and 77 K @panel ~c!# of the filaments near the edge of an Ag/Bi-2223 19-filament composite. The total thickness of the composite is 175 mm. The various labels are described in the text. formation during the following process resulting in thinner filaments near the center. The magnetic flux patterns were recorded in a transverse cross section, that is, in a plane perpendicular to the rolling direction of the composite with magnetic fields applied parallel to the rolling direction. This geometry does not give information on the variation of superconducting properties along the transport current direction ~i.e., the rolling direction!. However, it yields directly the superconducting morphology of the cross section through which the transport current has to flow. Figure 1 shows the magnetic flux patterns at 30 and 77 K, respectively, in 855 G associated with the three filaments near the edge of the tape together with the corresponding SEM image. The bright regions in the SEM image @Fig. 1~a!# are the silver matrix which has an overall crosssection thickness of 175 mm. The cross section is characterized by a variety of microstructural nonuniformities, namely second phase particles ~labeled ‘‘S’’!, irregularities in the alignment of the grain colonies ~labeled ‘‘G’’!, platelike outgrowths into the silver matrix ~labeled ‘‘OG’’! and pullouts generated in the polishing process ~labeled ‘‘P’’!. The second phase particles contain mostly ~Ca,Sr!2CuO3 , ~Ca,Sr!14Cu24O41 , and CuO. In the flux images @Figs. 1~b! and 1~c!# bright areas correspond to high levels of local field and dark areas to low local field levels. Low local fields at the sample surface are caused by effective shielding of the applied field by the superconductor, i.e., these areas constitute zones of high local critical current. The nonuniformities in the microstructure cause characteristic features in the flux patterns. Misoriented grain colonies give rise to sections of very weak critical current that effectively decouple different parts of the filament. This is particularly obvious near the middle of the left filament ~G1, G4!. The misoriented Bi-2223 colonies show up as light gray bands in the SEM image. Since these colonies contain well-aligned phase pure Bi-2223 they exhibit good superconducting shielding causing dark bands Appl. Phys. Lett., Vol. 66, No. 10, 6 March 1995 FIG. 2. SEM image @panel ~a!# and magnetic flux patterns at 30 K @panel ~b! and 77 K ~panel ~c!# of the filaments near the center of an Ag/Bi-2223 19-filament composite. The total thickness of the composite is 175 mm. The various labels are described in the text. in the magnetic patterns. G1 is the dark region right above the bright band across the middle of the left filament and G4 is the narrow dark line interrupting that bright band. Since these colonies are misoriented by nearly 45° with respect to the overall texture of the filament there exists a transitional region above and below the colonies with strongly distorted texture causing a depression of I c . These regions are the bright bands in the flux image. Similar behavior occurs near G2 and G3. As discussed above the Ag/Bi-2223 interface has a positive influence on the structural and superconducting properties. The flux patterns allow for the first direct observation of this phenomenon. The lower tip of the middle filament is characterized by two ‘‘good’’ superconducting outer layers ~seen as well-aligned colonies in the SEM image! and a ‘‘weak’’ center. This weak center line extends throughout the entire filament and is interrupted only by misoriented colonies. Similar behaviors are observed near the bottom tip and the top left edge of the right filament. These images demonstrate that enhanced superconducting properties along the Ag/Bi-2223 interface also exist in multifilament composites which contain much thinner filaments ~as compared to monofilament tapes!. The degree of development of this sandwiched structure ~‘‘good’’ interfaces–‘‘weak’’ core! varies strongly among filaments, in particular the center section of the middle filament in Fig. 2 appears almost uniform with good current carrying capability. The origins for this variation have not been clarified yet; however, it is shown that the OPIT process can yield filaments with uniform superconducting properties in their cross sections. With increasing temperature critical currents in Bi-2223 composites decrease rapidly10 which causes a strong decrease in the observed magnetic flux patterns. Figure 1~c! shows the magnetic patterns at 77 K. This image has been amplified strongly ~as evidenced by the high level of the background noise! in order to yield a legible figure. We note that with increasing temperature the structure of the magnetic patterns stays essentially the same, that is, no new weak links appear with increasing temperature. This implies that a Welp et al. 1271 field of 855 G applied at low temperatures is strong enough to break all the weak links and that the effect of increasing temperature is merely a further weakening of these links. The field dependence of these patterns will be discussed in more detail elsewhere.11 Pullouts or second phase particles cause disturbances of the flux patterns only when they cluster as seen near the top of the right and left filaments in Fig. 1. The SEM image and the flux patterns at 30 and 77 K of the central area of the composite are shown in Fig. 2. The magnetic patterns are characterized by a platelike structure oriented along the Ag/Bi-2223 interface in a manner similar to the behavior of the edgestack. This is clearly visible in the two left and the far right filaments. The texture in this central part of the tape appears to be better developed than near the edges; the number of misaligned grain colonies which cause an interruption of the supercurrent in the filament appears to be reduced in the strongly deformed center stack. In addition to these features this cross section is characterized by two interconnects ~labeled ‘‘I’’! between the filaments. The flux image at 30 K @Fig. 1~b!# shows that the large interconnect ~I1! carries a supercurrent whereas the small interconnect ~I2! is decoupled. Even though the flux patterns near the large interconnect are somewhat diffused at 77 K, it appears ~by following the plates at the filament edges! that at this elevated temperature the large interconnect is superconducting. An important consideration in the design of superconducting power-transmission lines is the level of ac losses. Depending on the geometry of a composite conductor and the presence of longitudinal or transverse magnetic fields in addition to the self-fields due to a transport current, rather complex loss mechanisms develop12 in which the coupling between the filaments is a crucial parameter. In the special case of independent filaments it is expected that the ac losses ~at small field amplitudes! in a multifilamentary conductor decrease like the inverse of the filament number ~for constant superconducting cross section!.13 However, experimentally it is found14 that the ac losses are essentially independent of the number of filaments. This behavior can be caused by a sufficient number of superconducting interconnects which will cause a strong coupling between filaments yielding an effective monofilamentary conductor. In conclusion, using a high-resolution magneto-optical technique we have obtained magnetic flux patterns of the current carrying cross section of a multifilamentary Bi-2223 composite conductor at temperatures up to 77 K and fields of 855 G. In conjunction with the microstructure determined 1272 Appl. Phys. Lett., Vol. 66, No. 10, 6 March 1995 from electron microscopy this technique gives unique information on the superconducting morphology of the sample. The images show that misaligned Bi-2223 grain colonies cause an interruption of the supeconducting properties of the filaments. Direct images of the enhanced superconducting properties along the Ag/Bi-2223 interface and a depression in the interior of the filaments have been obtained. Due to the rapid decrease of the critical currents, the magnetic signal decreases rapidly with increasing temperature. However, the structure of the magnetic patterns, i.e., the superconducting granularity, does not increase in any sufficient way. Also, we imaged two interconnects between filaments one of which was found to carry a supercurrent in high fields and discuss its significance of ac losses. This work was supported by the U.S. Department of Energy, BES—Materials Science ~U.W., G.W.C.! and the Office of Energy Efficiency and Renewable Energy ~J.S.L., V.A.M.! under Contract No. W-31-109-ENG-38 and the NSF-Office of Science and Technology Centers under Contract No. DMR91-20000 ~D.O.G.!. 1 G. N. Riley, D. R. Parker, C. J. Christopherson, P. K. Miles, J. J. Pickett, S. E. Hughson, J. D. Schreiber, A. Polyanskii, A. Pashitskii, and D. C. Larbalestier, Physica C 235–240, 3407 ~1994!. 2 D. C. Larbalestier, X. Y. Cai, Y. Feng, H. Edelman, A. Umezawa, G. N. Riley, Jr., and W. L. 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