SESSION R5: PROCESSING OF DEPOSITS, BSCCO, AND NEW MATERIALS
Chairs: David K. Christen and Dean E. Peterson
Wednesday Afternoon, April 2, 1997
Salon 15
1:30 PM R5.1
HIGH Jtex2html_wrap_inline105 Ag/Bi-2223 COMPOSITE CONDUCTORS: THE IMPORTANCE OF REACTION-INDUCED TEXTURE, Nazarali Merchant, Argonne National Laboratory, Chemical Tech Division, Argonne, IL; Stephen E. Dorris, Argonne National Laboratory, Dept of Energy Technology, Argonne, IL; Victor A. Maroni, Albert K. Fischer, Argonne National Laboratory, Chemical Technology Div, Argonne, IL.

It is well known that strong preferential c-axis texturing of Bi-2223 grains in Ag-clad Bi-2223 composite conductors plays a dominant role in the attainment of high Jtex2html_wrap_inline105 at 77 K and zero field. The mechanisms producing this texture are still not fully elucidated. Some researchers claim that deformation induced texture (DIT) is a key contributor, while others have shown that reaction induced texture (RIT) is the dominant mechanism. In this paper we intend to present an assessment of existing literature on this subject which suggests that both mechanisms may be important in obtaining good texture. Our results indicate that the dominant mechanism of texturing is also a function of the initial phase assemblage in the powder that goes into the silver tube before deformation processing. Tapes that exhibit appreciable RIT usually have the highest Jtex2html_wrap_inline105's because the liquid phase generated during heat treatment enhances grain growth and heals cracks that form during deformation processing.
tex2html_wrap_inline111Work sponsored by the U.S. Department of Energy (DOE), Energy Efficiency and Renewable Energy, as part of a DOE program to develop electric power technology under Contract W-31-109-ENG-38.

1:45 PM R5.2
TEXTURE AND PHASE DEVELOPMENT IN Ag-SHEATHED (Bi,Pb)tex2html_wrap_inline113Srtex2html_wrap_inline113Catex2html_wrap_inline113Cutex2html_wrap_inline119Otex2html_wrap_inline121 TAPES, Yuan L. Wang, Lijun Wu, Yimei Zhu, M. Suonaga, Brookhaven National Laboratory, Dept of Applied Science, Upton, NY; T. R. Thurston, Brookhaven National Laboratory, Dept of Physics, Upton, NY.

Texture and phase development for Bi(2212) to Bi(2223) conversion in powder-in-tube processed Bi(2223) tapes were investigated utilizing in situ transmission x-ray diffraction and ex-situ TEM techniques. It was found that Bi(2212) begins to develop texture at temperatures as low as tex2html_wrap_inline123750tex2html_wrap_inline125C. Bi(2212) developed texture rapidly for several hours, accompanied by rapid grain growth, upon raising the temperature to typical processing temperatures, and then slowed down dramatically, with much of the texture developing before the formation of Bi(2223). The degree of texture attained after long heating times was found to be temperature dependent, with higher temperatures generally producing better texture but not necessarily better transport properties. Briefly heating a sample near the Bi(2212) melting point can dramatically increase the texture, but such heating usually results in less Bi(2223) content. Finally, cooling rate was found to be related to the phase content and transport properties of a sample. These results and their implications for improving processing conditions are discussed.
tex2html_wrap_inline111Research supported by the U.S. Department of Energy, Division of Materials Sciences, and Office of Energy Efficiency and Renewable Energy under Contract No. DE-AC02-76CH00016.

2:00 PM R5.3
THE USE OF OXYGEN GRADIENTS AS A TEXTURING MECHANISM DURING ISOTHERMAL MELT PROCESSING OF BI-2212 SUPERCONDUCTORS., Terry G. Holesinger, John F. Bingert, Los Alamos National Laboratory, MST-6, Los Alamos, NM; J. Yates Coulter, Los Alamos National Laboratory, Superconductivity Tech Ctr, Los Alamos, NM; Jeffrey O. Willis, Los Alamos National Laboratory, MST-STC, Los Alamos, NM.

Isothermal melt processing (IMP) has shown itself to be a successful technique for processing Bi-2212 superconductors with high critical current densities. One of the interesting aspects of IMP is the oxygen gradient that occurs within the sample during the oxidation step. It is shown that this oxygen gradient can be used as a texturing mechanism to form uniaxial texture in large scale Bi-2212 conductors. In terms of bulk Bi-2212 conductors, this has lead to improved self-field critical current values and improved performance in applied fields. With the appropriate conductor design, the oxygen gradient can be used to help texture oxide powder-in-tube (OPIT) conductors.

2:15 PM R5.4
OXYGEN EXCHANGE IN Ag-SHEATHED Bi-2223 TAPES, Mario Quilitz, Wilfried Goldacker, Forschungszentrum Karlsruhe, Inst fur Technische Physik, Karlsruhe, GERMANY.

The exchange of oxygen in the Bi-2223 phase has a great influence on the conditions of phase formation and on the superconducting properties of the high temperature superconductors. It is well known that the oxygen stoichiometry has a distinct effect on the detect chemistry and therefore via the defect electron concentration on the electrical properties of the 2223 phase. It is as well known that the oxygen stoichiometry has a big influence on the kinetics of HTSc. The effect of oxygen exchange on the phase formation and the critical currents in Ag-sheathed Bi-2223 tapes was investigated via thermogravimetric analysis. The study of the oxygen uptake and the release were performed via a chemical relaxation process during which the change in weight was monitored with time after a fast change in atmosphere. For both pore Ag and a Ag-alloy with 2tex2html_wrap_inline129 Mg the oxygen exchange was studied at various temperatures. The oxygen uptake is different with regard to whether the oxygen exchanges through the open ends of the tape where the superconductor is in direct contact with the surrounding gas-phase or whether the exchange takes place via the lateral faces of the tape which means through the sheath material. Methods for a separated analysis of both processes are discussed. The different exchange properties with different sheath material are discussed as well as its effect on the phase formation and the final critical currents in the tapes.

2:30 PM R5.5
STRUCTURE AND PROPERTIES OF [001] TWIST BOUNDARIES IN Bi/2212 BICRYSTALS, Yimei Zhu, Qiang Li, Y. N. Tsay, Masaki Suenaga, Brookhaven National Laboratory, Dept of Applied Science, Upton, NY.

[001] twist boundaries account fortex2html_wrap_inline13180tex2html_wrap_inline129 of total grain boundaries in c-axis aligned polycrystalline Bi/2212 tapes, which are one of the most promising high temperature superconductors for large scale applications to date. Systematic studies of these important [001] twist boundaries were fabricated with a wide range of twist angles (0tex2html_wrap_inline125-180tex2html_wrap_inline125). The resistance and current-voltage characteristics were measured simultaneously at various temperatures and magnetic fields. The boundary structures were then characterized with TEM, using high-resolution imaging and image simulation incorporating with charge distribution, nano-probe electron energy-loss spectroscopy and energy dispersive x-ray spectroscopy, and strain-field analysis. Contrary to the conventional wisdom, all these twist boundaries, regardless of their twist angle, carried the same critical current as their constituent single crystals at magnetic field up to 9 tesla at low temperatures. The absence of the weak-link behavior of the [001] twist boundaries can be attributed to the variation of elastic properties of the (001) layers (the soft-bonding of the BiO bilayer at the boundaries and the rigid interlayer-bonding of the CuOtex2html_wrap_inline113 layers across the boundaries), to the local Bi/2223 structure, and to stoichiometric chemical composition including oxygen/hole concentration of the grain boundaries. Our recent work on the structure and properties of various tilt boundaries in Bi/2212 bicrystals will also be presented.
tex2html_wrap_inline111This work was supported by the U.S. Dept. of Energy, Division of Materials Sciences, Office of Basic Energy Science, under Contract No. DE-AC02-76CH00016.

2:45 PM R5.6
SIGNIFICANCE OF COOLING RATE ON MICROSTRUCTURE AND TRANSPORT PROPERTIES OF Ag-SHEATHED BSCCO(2223) TAPES, N. Vasanthamohan, J. P. Singh, Argonne National Laboratory, Dept of Energy Technology, Argonne, IL.

To maximize the current-carrying capacity of Ag-sheathed Bitex2html_wrap_inline143 superconducting tapes, a two step cooling procedure was developed. Monolithic and wire-in-tube tapes at 825tex2html_wrap_inline125C in 8tex2html_wrap_inline129 Otex2html_wrap_inline113 (balance Ntex2html_wrap_inline113) in two 50-h cycles, for a total of 100 h, with one intermediate pressing at 1 GPa for 5 s. Subsequently, the tapes were cooled by the two-step cooling procedure. The first cooling step was used to control the solidification of the partial melt to produce a dense microstructure with large grains, while the second cooling step maintained phase purity. The results indicate a pronounced effect of cooling rate on 2223 content during the first 50 h of sintering. At longer sintering times, the effect of cooling rate on 2223 content was minimal. On the other hand, the effect of cooling rate on critical current (Itex2html_wrap_inline105) is quite pronounced even after 100 h of sintering. This strong influence of cooling rate on Itex2html_wrap_inline105 is attributed to microstructural changes that occur during cooling.
tex2html_wrap_inline111Work at Argonne National Laboratory is supported by the U.S. Department of Energy, Pittsburgh Energy Technology Center, under Contract W-31-109-Eng-38.

3:30 PM R5.7
ANNEALING EFFECTS AND THERMOSTABILITY OF Ba-Ca-Cu-O COMPOUNDS, Yong Cao, Univ of Houston, TCSUH, Houston, TX; Ching-Wu Chu, Univ of Houston, Dept of Physics, Houston, TX; Z. L. Du, Yanyi Sum, Li Gao, Univ of Houston, TCSUH, Houston, TX; Yuyi Xue, Univ of Houston, Dept of Physics, Houston, TX.

The high-pressure synthesized new 126K superconducting phase in Ba-Ca Cu-O is successfully identified. Although the superconducting transition temperature Ttex2html_wrap_inline105 of (Cu,C)-1234 is about 117K, and that of (Cu,C) 1223 can be raised from 67K to tex2html_wrap_inline123120K, which is not far away from that of the new superconducting phase, their annealing effects and thermostability are quite different from the new phase. For example, after annealed at 300tex2html_wrap_inline125C in Ar, the Ttex2html_wrap_inline105 of the 126K-phase can be suppressed to tex2html_wrap_inline12380K, while the Ttex2html_wrap_inline105 of (Cu,C)-1223 increases to 70K and that of (Cu,C)1234 barely changes. Ttex2html_wrap_inline105 variations are systematically studied under different thermo-equilibrium conditions. While no significant decomposition was observed in (Cu,C)-1223 anal (Cu,C)-I234 when annealing temperature is lower than 600tex2html_wrap_inline125C, the new superconducting phase is not even stable at room temperature, especially with moisture. It can decay into another superconducting phase with Ttex2html_wrap_inline175 90K, while significant change in x-ray diffraction pattern appears at the same time.

3:45 PM R5.8
RHENIUM INFLUENCE ON THE SYNTHESIS OF SUPERCONDUCTING Hgtex2html_wrap_inline177Retex2html_wrap_inline179Batex2html_wrap_inline113Catex2html_wrap_inline113Cutex2html_wrap_inline119Otex2html_wrap_inline187 CERAMICS AND THICK FILMS, S. Pinol, CSIC, Inst de Ciencia de Matls de Barcelona, Bellaterra, SPAIN; Agustin Sin, Albert Calleja, CSIC, Inst de Ciencia de Materials de Barcelona, Bellaterra, SPAIN; Xavier Obradors, CSIC, Inst de Ciencia de Matls de Barcelona, Bellaterra, SPAIN; Josep Fontcuberta, CSIC, Inst de Ciencia de Materials de Barcelona, Bellaterra, SPAIN; Ferran Espiell, Univ de Barcelona, Dept of Engr Quinica i Metallurgia, Barcelona, SPAIN.

We have prepared high quality ceramics of the superconducting phase Hgtex2html_wrap_inline189Retex2html_wrap_inline191Batex2html_wrap_inline113Catex2html_wrap_inline113Cutex2html_wrap_inline119Otex2html_wrap_inline187 with a critical temperature onset of 138 K and zero resistance at 130 K. The superconductors were prepared using precursor powders of Batex2html_wrap_inline113Catex2html_wrap_inline113Cutex2html_wrap_inline119Otex2html_wrap_inline207 mixed with stoichiometric additions of ReO2 and HgO. We have utilized these ceramics for the preparation of thick film superconductors by the vacuum-sealed quartz technique. Ceramic pellets were obtained by solid state reaction of the precursors inside a quartz tube at 900tex2html_wrap_inline125C. We have studied the influence of different thermal treatments in the kinetics of the reaction. Different Re compositions were explored in order to optimize the purity of the 1223 phase. Only a very narrow Re composition was found to be appropriate to obtain single phases. Cell parameters and composition were characterized using a SQUID magnetometer, and AC susceptometer and electrical resistivity. We have studied the vapor-solid reaction of the Hg-vapors with a Retex2html_wrap_inline179Batex2html_wrap_inline113Catex2html_wrap_inline113Cutex2html_wrap_inline119Otex2html_wrap_inline219 thick films precursor (tex2html_wrap_inline221m thickness) deposited by spray techniques on different metallic and ceramic substrates (Cr, Altex2html_wrap_inline113Otex2html_wrap_inline119, SrTiOtex2html_wrap_inline119). We have placed the samples in a sealed quartz tube together with stoichiometric Hg-Re-Ba Ca-Cu-O pellets in order to maintain an appropriate Hg-vapor pressure. Then the tubes were introduced rapidly into a preheated furnace at 900tex2html_wrap_inline125C for a few minutes and quickly cooled at room temperature by quenching in air. Superconducting Hg-1223 grains with c-axis oriented perpendicular to the substrate were identified by Scanning Electron Microscopy and EDX analysis. Homogeneity and composition of the thick film grains depend strongly on the time thermal treatment.

4:00 PM R5.9
DEVELOPMENT OF HIGH-CURRENT YBatex2html_wrap_inline113Cutex2html_wrap_inline119Otex2html_wrap_inline235 COATED CONDUCTORS ON ROLLED-Ni SUBSTRATES, Mariappan Paranthaman, Oak Ridge National Laboratory, Dept of Chemical & Analytical Science, Oak Ridge, TN; F. A. List, Oak Ridge National Laboratory, Solid State Div, Oak Ridge, TN; David P. Norton, Oak Ridge National Laboratory, Oak Ridge, TN; Amit Goyal, Oak Ridge National Laboratory, Metals & Ceramics Div, Oak Ridge, TN; E. D. Specht, David K. Christen, D. M. Kroeger, John D. Budai, Qing He, Oak Ridge National Laboratory, Solid State Div, Oak Ridge, TN; Dominic F. Lee, Oak Ridge National Laboratory, Metals & Ceramics Div, Oak Ridge, TN; P. M. Martin, Oak Ridge National Laboratory, Oak Ridge, TN.

High Current YBatex2html_wrap_inline237 (referred to as YBCO) Coated Conductors were fabricated with a layer sequence of YBCO/YSZ/CeOtex2html_wrap_inline113/Ni. The cube (100) texture in the starting Ni substrates was obtained by cold-rolling followed by recrystallization. The CeOtex2html_wrap_inline113 and YSZ films were grown epitaxially on the textured Ni substrates using electron beam evaporation and rf magnetron sputtering techniques. The YBCO films were then grown by pulsed laser deposition. The biaxial texture in the YBCO layer is over 90tex2html_wrap_inline129. A high transport critical current density of 7.8 x 105 tex2html_wrap_inline245/cmtex2html_wrap_inline247 at 77 K was obtained on 0.7 tex2html_wrap_inline249m thick YBCO films in zero field. The effect of buffer layer thicknesses will be discussed. We also recently demonstrated that over 6 cm long buffered substrates with good biaxial texture can be obtained using the electron beam evaporation technique. Research was sponsored by the Division of Materials Sciences, Office of Basic Energy Sciences and Office of Energy Efficiency and Renewable Energy, Office of Utility Technology-Superconductivity Program, performed at ORNL, managed by Lockheed Martin Energy Research Corporation for the U.S. Department of Energy under contract DE-AC05-96OR22464.

4:15 PM R5.10
R.F. SPUTTERING OF BIAXIALLY-TEXTURED YSZ BUFFER LAYER ON ANGULAR ORIENTED METALLIC SUBSTRATE, Gregory Kozlowski, Cary Farlow, Jason Hundley, Wright State Univ, Dept of Physics, Dayton, OH; C. Varanasi, Univ of Dayton, Research Inst, Dayton, OH; Iman Maartense, Rama Nekkanti, E. K. Moser, Rand Biggers, Air Force Wright Laboratory, WL/MLPO, Wright Patterson AFB, OH; Charles E. Oberly, Air Force Wright Laboratory, WL/POOX, Dayton, OH; Tim L. Peterson, Air Force Wright Laboratory, Wright Patterson AFB, OH; Venkat Selvamanickam, Intermagnetics General Corp, Latham, NY; Ana Ivanova, SUNY-Albany, Albany, NY; Alain E. Kaloyeros, SUNY-Albany, Dept of Physics, Albany, NY.

Biaxially-textured YSZ buffer layers were fabricated by a modified RF sputtering technique on Hastelloy C276 substrates. Our YSZ films had the strongest (200) preferred orientation when the films were grown at an RF power of 300 W and an Ar-2tex2html_wrap_inline129Otex2html_wrap_inline113 pressure of 10tex2html_wrap_inline255 Torr while they were tilted at approximately 70tex2html_wrap_inline125 from the horizontal plane and at a target-to-substrate distance of approximately 2 cm. Substrates of Hastelloy C276 were polished to a mirror finish using aluminum oxide lapping powders. To characterize the in-plane texturing of the YSZ buffer layers, x-ray polo figure measurements using the Schultz reflection method were carried out. The full width at the half-maximum (FWHM) of the YSZ (111) peak, as a measure of the alignment of the YSZ grains, wa about 25tex2html_wrap_inline125 at best. Next, YBatex2html_wrap_inline113Cutex2html_wrap_inline119Otex2html_wrap_inline265 (YBCO) films deposited on YSZ/Hastelloy C276 by laser ablation or MOCVD technique. The x-ray rocking curve FWHM for the YBCO (013) peak was 13tex2html_wrap_inline125 on a YSZ buffer layer which was considerably less well textured than the best result noted above. The superconducting properties of the YBCO films will be discussed as a function of sputtering parameters.

4:30 PM R5.11
LARGE AREA DEPOSITION OF YBCO-FILMS BY PULSED-LASER DEPOSITON ON VARIOUS SUBSTRATES, Bernd Schey, Wolfgang Biegel, Gebbhard Ostreicher, Marcus Kuhn, Univ Augsburg, Dept of Physics, Augsburg, GERMANY; Bernd Stritzker, Univ Augsburg, Inst of Physics, Augsburg, GERMANY.

Fault Current Limiters (FCL) on the basis of HTS thin film material require large areas of YBatex2html_wrap_inline113Cutex2html_wrap_inline119Otex2html_wrap_inline265 (YBCO) films with homogeneous superconducting properties. Pulsed Laser Deposition (PLD) is used to deposit YBCO on two different kinds of substrates (CeOtex2html_wrap_inline113-buffered sapphire and biaxial textured YSZ buffer on polycrystalline YSZ) with a size up to 7 x 20 cmtex2html_wrap_inline247. YBCO films with constant thickness are produced by a special PLD setup with a 8 cm line-focus on a cylindrical target and substrate scanning perpendicular to it. The spatial variation of the critical current density jtex2html_wrap_inline105 (77 K) and the transition temperature Ttex2html_wrap_inline105 over the area of 7 x 20 cmtex2html_wrap_inline247 was investigated by an inductive method. Small samples (1 x 1 cmtex2html_wrap_inline247) were used to study the influence of activated oxygen provided by an ion source during YBCO deposition.
Work supported by BMBF (13N6482) and Bayerische Forschungsstiftung FORSUPRA.

4:45 PM R5.12
YBatex2html_wrap_inline113Cutex2html_wrap_inline119Otex2html_wrap_inline291 COATED CONDUCTORS BY LIQUID PHASE EPITAXY USING BaFtex2html_wrap_inline113-ADDED OXIDE SOLUTION, Yasuji Yamada, ISTEC, Superconductivity Research Lab, Nagoya, JAPAN; Junichi Kawashima, Yusuke Niiori, Izumi Hirabayashi, Shoji Tanaka, ISTEC, Nagoya, JAPAN.

YBCO-coated conductors on yttria stabilized zirconia (YSZ) and SrTiOtex2html_wrap_inline119 (STO) single crystalline fibers of 0.4 mm in diameter have been formed by low temperature liquid phase epitaxy using BaFtex2html_wrap_inline113 added oxide flux. Since BaFtex2html_wrap_inline113 addition make the crystallization temperature lower down to 920tex2html_wrap_inline125C, reaction between the substrate material and the flux is suppressed enough to steadily form YBCO film coating the fibers. YBCO coated conductors were prepared by dipping the fiber that had been pre-coated by a YBCO thin film by laser ablation as a seed layer of the solution growth. The growth temperature and time were 925tex2html_wrap_inline125C for 5 min. The thickness of the film was about 5 tex2html_wrap_inline249m. Although the YSZ fibers grown along [100] are almost cylindrical, c-axis oriented YBCO film grows on the round face the c-axis parallel to the <100> direction of the base fiber. The films grown on the STO fiber have rather smooth surface maybe due to the facet faces formed on the surface of the fiber.
YBCO coated fibers show superconductivity at about 90 K. Magnetic field dependence shows gradual decrease of critical current at 77 K, indicating that there is no weak-linked grain boundaries in the film. This work was supported by NEDO.



Go Back

| Site Map | What's New | MRS Home | Comments | Search | Contacts |
| Society Information | Meetings | Membership | Publications | Marketing Opportunities |

Copyright©1999
Materials Research Society
506 Keystone Drive, Warrendale, PA 15086-7573 USA
Phone: 724 779-3003, Fax: 724 779-8313
, webmaster@mrs.org