1067 1 Fabrication and Characterization of Multi-layer YBCO Coated Conductors on a Curved Surface Y.L. Cheung, E.F. Maher, J.S. Abell and I.P. Jones Abstract— Biaxially textured YBCO films and various buffer layers were prepared in situ on rotating cylindrical surfaces using highly cube textured pure Ni and Ni-5at%W RABiTS tapes by pulsed laser deposition (PLD). The superconducting and crystallographic properties of the curved composite were similar to those achieved on flat surfaces. The cube textures of the curved architecture were characterized by electron back-scattered patterns (EBSP). Cross-sectional TEM and Scanning transmission electron microscopy (STEM) were used to determine the chemical analysis, diffusion characteristics, microstructures and interfaces of the curved multilayer samples. Index Terms—coated conductors, EBSP, STEM, YBCO I. INTRODUCTION O BTAINING higher JE (Engineering Current Density) and good performance in high magnetic field are parts of major research work in superconducting wires or coil applications. Multi-YBCO layers and STO insulating layers have been successfully deposited on the standard buffer layer architecture of RABiTS (CeO2/YSZ/CeO2) by pulsed laser deposition on a curved Ni substrate to demonstrate an innovative integrated fabrication technology in High Temperature Superconducting coil applications [1-3]. This approach is proposed to use a combination of thin film deposition and patterning techniques in order to prepare a multi-turn, multi-layered cylindrical coil (coated conductor cylinder) without the requirement of producing long lengths of coated conductor tape. If this novel technology is successful, only one layer of base substrate would be required to provide the initial texture, thus the cost will be dramatically reduced and JE will be significantly increased by proportionately increasing the YBCO cross-sectional area. Moreover, producing a coil is simply by a multi-layer in situ deposition sequence onto a rotating cylindrical former [2-3]. It will overcome the requirements of reproducible manufacture of kilometre lengths within a vacuum chamber. Manuscript received October 5, 2004. Y.L. Cheung is with the School of Metallurgy and Materials, The University of Birmingham, Edgbaston, Birmingham, B15 2TT, UK (corresponding author phone: 44-121-4145209; e-mail: ylc263@bham.ac.uk). E.F. Maher is with Coated Conductor Consultancy Ltd 4 High Street, Watlington, Oxon, OX9 5PS, UK (e-mail: enquires@3-3s.co.uk). J.S. Abell and I.P. Jones are with the School of Metallurgy and Materials, The University of Birmingham, Edgbaston, Birmingham, B15 2TT, UK (email: j.s.abell@bham.ac.uk, i.p.jones@bham.ac.uk). Electron back-scattered diffraction patterns have been used to study the cube architecture of curved coated conductor samples. On the other hand, the detailed interface microstructure and chemical analysis of curved coated conductor samples has been characterized by scanning transmission electron microscopy (STEM) in this paper. II. EXPERIMENTAL YBCO multi-layer and buffer layers were grown on a curved Ni RABiTS substrate from Oxford Instruments or curved Ni-5at%W RABiTS substrates from IFW Dresden. All layers were prepared in situ by a Lambda Physik LPX200i Excimer laser running at 248nm (KrF). A special rotating cylindrical heated former (3cm diameter) was used in this research in order to produce in situ formation of multi-turn and multi-layered HTS coils. The deposition parameters were chosen to be the same as for optimised flat tapes [3]. The target-substrate distance was 5.5 - 6cm, laser fluence of 1.5 – 2 J/cm2, substrate temperature of 780oC, oxygen pressure of 0.6mbar, cooling down at 10oC/min in 700mbar oxygen after the ablation. To reduce the possibility of substrate oxidation and to remove oxide on the substrate, 0.15 mbar of reducing gas: 4% H2 in argon, was introduced to the chamber during heating of the substrate. Electron Backscattered Diffraction (EBSD) patterns were obtained from JEOL 840A Scanning Electron Microscope with an Oxford Instruments INCA detector. The diffraction pattern can be used to measure the crystal orientation and the grain boundary misorientations which are indexed from the Kikuchi bands. To prepare the cross-sectional TEM samples, a Gatan model 691 Precision Ion Polishing System (PIPS) was used to mill the sample. During ion milling, the ion-milling holder was rotated and two ion guns were used. A typical ion milling condition was at a 10o tilt angle and 5keV ion beam energy. When coloured fringes were observed, the ion milling condition was changed into an ion polishing procedure. The ion polishing condition was at a 8o tilt angle and 3keV of ion beam energy. The electron micro-images were observed on a transmission electron microscope (Model Tecnai F20, FEI) with a field emission gun (FEG) and energy dispersive spectrometer which can operate in scanning mode as Scanning Electron microscope (STEM). 1067 2 III. RESULTS AND DISCUSSION A. Electron Backscatter Diffraction Standard buffer architecture (CeO2/YSZ/CeO2) were grown both on curved pure Ni and Ni-5at%W tapes using the same parameters in order to determine the surface texture quality of that buffer architecture. Grain boundary data from those two samples are shown in Fig. 1 and Fig. 2. For the buffered Ni-W tape, grains were significantly smaller than the grains on pure Ni tape. Furthermore, more grains were misoriented between 2-10 degree compared to the buffered Ni, which indicated a better cube texture in order to grow good quality YBCO layers on Ni-W tapes[5]. Fig. 2. Grain boundary data measured by EBSD from the final CeO 2 layer deposited on curved buffered Ni-5%W. (Up) Grain boundary positions superimposed on the pattern quality image. (Down) The boundaries are colour coded according to the histogram of misorientation angle. Fig. 1. Grain boundary data measured by EBSD from the final CeO 2 layer deposited on curved buffered Ni. (Up) Grain boundary positions superimposed on the pattern quality image. (Down) The boundaries are colour coded according to the histogram of misorientation angle. B. Scanning Transmission Electron Microscopy Triple YBCO layers were grown on a buffered curved Ni substrate using SrTiO3 insulating layers. High-resolution images and diffraction patterns of the interfaces were presented in a previous paper from a Tecnai TEM [3]. Further microanalysis of the sample is discussed here by STEM operation with the same TEM. TEM bright field image and STEM dark field images of the triple YBCO layers are shown in Fig. 3 and Fig. 4. No secondary phase particles or reaction phases were found within the films. However, from Fig. 3, the surface of the sample showed outgrowth formation (white arrows) with approximately 300nm in diameter. It is evident that the outgrowth formation was due to the surface roughness of the second YBCO layer and second STO insulating layer. Moreover, droplet shapes of porosity (black arrows) were found in the YBCO layer as shown in Fig. 3 and Fig. 4. The thicker the YBCO layer, the more the pores have been observed. Porosity content in YBCO is related to the film thickness [6]. 1067 3 st 1 YBCO 70 nd STO STO 2 YBCO rd 3 YBCO Ba 60 counts 50 40 Cu 30 O 20 10 Sr 0 Ti 0 200 400 600 800 1000 1200 position(nm) Fig. 3. Cross-sectional transmission electron micrograph of triple YBCO layers on curved buffered Ni tapes. Outgrowths are indicated by white arrows and pores are indicated by black arrows. Fig. 5. STEM quantmap from the first YBCO layer to third YBCO layer. clean. It proves that there was no significant diffusion between the YBCO layers and STO insulating layers. SrTiO3 is a good diffusion barrier and insulating layer in this research. Moreover, it can provide a very good template for patterning YBCO layers on curved surface. IV. CONCLUSIONS 200nm Fig. 4. Dark field STEM image of triple YBCO layers on curved buffered Ni tapes. Black arrow indicates the porosity in the first YBCO layer. Sharp and cube EBSD patterns of CeO2/YSZ/CeO2 on curved Ni and NiW tapes were successfully acquired. The grains on pure Ni tapes had large misorientation; however, the misorientation of the grains on NiW tapes were mostly between 2-10 degree which provides a good template for growing YBCO layers. Outgrowths and pores were observed in the YBCO layers. TEM micrographs showed that the occurrence of pores and surface roughness were dependent on YBCO thickness. STEM quantmap linescan showed that there was no significant diffusion between the YBCO layers and STO insulating layers. STO is a good diffusion barrier and insulating layer for separating YBCO layers in this research. ACKNOWLEDGMENT A STEM quantmap linescan was acquired from the first YBCO layer to the third YBCO layer shown in Fig. 5 which performs a quantitative analysis at each point on the line. The Y signal is relatively low and has been omitted from Fig. 5 for the sake of clarity. The elements showed even counts in each layer and the interfaces between the layers were sharp and The authors gratefully acknowledge Dr. B. Holzapfel and Dr. J. Eickemeyer of IFW-Dresden for providing the Ni5at%W tapes and helpful discussions. The authors would like to thank R.I. Chakalova for preparing the samples on Ni tapes. 1067 4 REFERENCES [1] [2] [3] [4] [5] [6] E.F. Maher, J.S. Abell, R.I. Chaklova, Y.L. Cheung, T.W. Button and P. Tixadov, “Multi-layer coated conductor cylinder – an alternative approach to superconducting coil fabrication,”Supercon. Sci. Tech., submitted for publication. Y.L. Cheung, G. Passerieux, I.P. Jones and J.S. Abell, “Microstructural study of multilayer YBCO on a curved Ni surface,”Inst. Phys. Conf., Ser. No 179: Section 2, 2003, pp. 107-110. Y. L. Cheung, R.I. Chakalova, J.S. Abell, T.W. Button and E.F. Maher, “Growth of multi-layer YBCO on a curved Ni surface,” presented at the 6th European Conference on Applied Superconductivity 2003. R.I. Chakalova, C. Cai, T. Woodcock, T.W. Button, J.S. Abell and E.F. Maher, “Fabrication and characterization of YBCO coated nickel-based tapes with various buffer layers,” Physica C, Vol. 372-376, Part 2, 2002, pp.846-850. J. Eickemeyer, D. Selbmann, R. Optiz, H. Wendrock, E. Maher, U. 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