Soft-chemistry synthesis of Ba2Ca2Cu3Ox precursor and characterization of high-Tc Hg0.8Pb0.2Ba2Ca2Cu3O8+δ superconductor

T. BRYLEWSKI; K. PRZYBYLSKI; A. MORAWSKI; D. GAJDA; T. CETNER; J. CHMIST

doi:10.1007/s40145-016-0189-x

Journal of Advanced Ceramics 2016, 5(3): 185-196 https://doi.org/10.1007/s40145-016-0189-x

Research Article |

Open Access | Issue | Published: 29 June 2016

Soft-chemistry synthesis of Ba₂Ca₂Cu₃O_x precursor and characterization of high-T_c Hg_0.8Pb_0.2Ba₂Ca₂Cu₃O_8+δ superconductor

Show Author's Information Hide Author's Information T. BRYLEWSKI^{^a}(

), K. PRZYBYLSKI^{^a}, A. MORAWSKI^{^b}, D. GAJDA^{^c}, T. CETNER^{^b}, J. CHMIST^{^d}

^a AGH University of Science and Technology, Faculty of Materials Science and Ceramics, Al. Mickiewicza 30, 30-059 Krakow, Poland

^b Institute of High Pressure Physics of the Polish Academy of Sciences, Superconductor Laboratory NL-6, ul. Prymasa Tysiąclecia 98, 00-893 Warsaw, Poland

^c International Laboratory of High Magnetic Fields and Low Temperatures, ul. Gajowicka 95, 53-421 Wroclaw, Poland

^d AGH University of Science and Technology, Faculty of Physics and Applied Computer Science, Al. Mickiewicza 30, 30-059 Krakow, Poland

Keywords:

microstructure, superconductor, EDTA gel process, secondary phase

Cite this article:

BRYLEWSKI T, PRZYBYLSKI K, MORAWSKI A, et al. Soft-chemistry synthesis of Ba₂Ca₂Cu₃O_x precursor and characterization of high-T_c Hg_0.8Pb_0.2Ba₂Ca₂Cu₃O_8+δ superconductor. Journal of Advanced Ceramics, 2016, 5(3): 185-196. https://doi.org/10.1007/s40145-016-0189-x

Download citation

EndNote(RIS)

BibTeX

531

Views

Downloads

Citations

Crossref

N/A

WoS

Scopus

CSCD

Abstract Full text About this article

Abstract

The paper describes the sol–gel process applied to synthesize a mercury-free Ba₂Ca₂Cu₃O_x precursor and the physicochemical properties of an Hg_0.8Pb_0.2Ba₂Ca₂Cu₃O_8+δ high-temperature superconductor (HTS) polycrystalline sample. The Ba₂Ca₂Cu₃O_x precursor with desired chemical and phase compositions was obtained using EDTA gel process followed by decomposition and calcination under optimized conditions. An Hg_0.8Pb_0.2Ba₂Ca₂Cu₃O_8+δ superconductor with a fine-grained microstructure, composed predominantly of the (Hg,Pb)-1223 phase in the form of plate-like crystallites or oval grains and with advantageous magnetic properties (T_c(on) = 129.2 K, ΔT_c = 6.5 K), was synthesized using the high-pressure crystallization method. At 20 K and 1 T, the critical current density of the studied sample was approximately 26 A/mm², while at 4 K and 1 T it increased to 155 A/mm². The high volume fraction of the (Hg,Pb)-1223 phase (89.1%) in the high-T_c sample was associated with the low value of the average copper valence (2.11) in the calcinated Ba₂Ca₂Cu₃O_x precursor. Small amounts of non-superconducting secondary phases—BaCuO₂, CaO, CaHgO₂, CuO, Ca₂CuO, BaPbO₃—were also identified within the microstructure of Hg_0.8Pb_0.2Ba₂Ca₂Cu₃O_8+δ.

Full text

Abstract

Full text

Outline

About this article

Soft-chemistry synthesis of Ba₂Ca₂Cu₃O_x precursor and characterization of high-T_c Hg_0.8Pb_0.2Ba₂Ca₂Cu₃O_8+δ superconductor

Show Author's information Hide Author's Information T. BRYLEWSKI^{^a}(

), K. PRZYBYLSKI^{^a}, A. MORAWSKI^{^b}, D. GAJDA^{^c}, T. CETNER^{^b}, J. CHMIST^{^d}

^a AGH University of Science and Technology, Faculty of Materials Science and Ceramics, Al. Mickiewicza 30, 30-059 Krakow, Poland

^b Institute of High Pressure Physics of the Polish Academy of Sciences, Superconductor Laboratory NL-6, ul. Prymasa Tysiąclecia 98, 00-893 Warsaw, Poland

^c International Laboratory of High Magnetic Fields and Low Temperatures, ul. Gajowicka 95, 53-421 Wroclaw, Poland

^d AGH University of Science and Technology, Faculty of Physics and Applied Computer Science, Al. Mickiewicza 30, 30-059 Krakow, Poland

Abstract

Keywords: microstructure, superconductor, EDTA gel process, secondary phase

References(47)

[1]

Putilin

, Antipov

, Chmaissem

, et al. Superconductivity at 94 K in HgBa₂Cu0_4+δ. Nature 1993, 362: 226–228.10.1038/362226a0

DOI Google Scholar

[2]

Putilin

, Antipov

, Marezio

. Superconductivity above 120 K in HgBa₂Cu₂O_6+δ. Physica C 1993, 212: 266–270.10.1016/0921-4534(93)90588-H

DOI Google Scholar

[3]

Meng RL, Beauvais L, Zhang XN, et al. Synthesis of the high-temperature superconductors HgBa₂Cu₂O_6+δ and HgBa₂Ca₂Cu₃O_8+δ. Physica C 1993, 216: 21–28.

DOI Google Scholar

[4]

Schilling A, Cantoni M, Guo JD, et al. Superconductivity above 130 K in the Hg–Ba–Ca–Cu–O system. Nature 1993, 363: 56–58.

DOI Google Scholar

[5]

Schilling

, Jeandupeux

, Guo

, et al. Magnetization and resistivity study on the 130 K superconductor in the Hg–Ba–Ca–Cu–O system. Physica C 1993, 216: 6–11.10.1016/0921-4534(93)90626-2

DOI Google Scholar

[6]

Chu CW, Gao L, Chen F, et al. Superconductivity above 150 K in HgBa₂Ca₂Cu₃O_8+δ at high pressures. Nature 1993, 365: 323–325.

DOI Google Scholar

[7]

Schilling

, Jeandupeux

, Büchi

, et al. Physical properties of HgBa₂Ca₂Cu₃O₈ with T_c ≈ 133 K. Physica C 1994, 235–240: 229–232.10.1016/0921-4534(94)91355-2

DOI Google Scholar

[8]

Wagner JL, Radaelli PG, Hinks DG, et al. Structure and superconductivity of HgBa₂CuO_4+δ. Physica C 1993, 210: 447–454.

DOI Google Scholar

[9]

Lin CT, Yan Y, Peters K, et al. Flux growth Hg₁_-xRe_xBa₂Ca_n-1Cu_nO_2n+2+δ single crystals by self-atmosphere. Physica C 1998, 300: 141–150.

DOI Google Scholar

[10]

Sin A, Cunha AG, Calleja A, et al. Formation and stability of HgCaO₂, a competing phase in the synthesis of Hg₁_-xRe_xBa₂Ca₂Cu₃O_8+δ superconductor. Physica C 1998, 306: 34–46.

DOI Google Scholar

[11]

Kandyel E, Elsabawy KM. New 1201-Type (Hg,Se)-superconducting cuprate grown by sol–gel and sealed quartz tube synthesis. Physica C 2008, 468: 2322–2327.

DOI Google Scholar

[12]

Przybylski K, Morawski A, Łada T, et al. Synthesis and properties of (Hg₁_-xRe_x)Ba₂Ca₂Cu₃O_8+δ HTS single crystals and films obtained by high-pressure gas method. Physica C 2000, 341–348: 543–544.

DOI Google Scholar

[13]

Isawa

, Tokiwa-Yamamoto

, Itoh

, et al. Encapsulation method for the synthesis of nearly single-phase superconducting HgBa₂Ca₂Cu₃O_8+δ with T_c ≈135 K. Physica C 1994, 222: 33–37.10.1016/0921-4534(94)90111-2

DOI Google Scholar

[14]

Shao HM, Shen LJ, Shen JC, et al. Synthesis of single-phase HgBa₂Ca₂Cu₃O_8+δ superconductor. Physica C 1994, 232: 5–9.

DOI Google Scholar

[15]

Tokiwa-Yamamoto A, Isawa K, Itoh M, et al. Composition, crystal structure and superconducting properties of Hg–Ba–Cu–O and Hg–Ba–Ca–Cu–O superconductors. Physica C 1993, 216: 250–256.

DOI Google Scholar

[16]

Shao HM, Lam CC, Fung PC, et al. The synthesis and characterization of HgBa₂Ca₂Cu₃O_8+δ superconductors with substitution of Hg by Pb. Physica C 1995, 246: 207–215.

DOI Google Scholar

[17]

Lee S, Shlyakhtin OA, Mun M-O, et al. A freeze-drying approach to the preparation of HgBa₂Ca₂Cu₃O_8+x superconductor. Supercond Sci Technol 1995, 8: 60–65.

DOI Google Scholar

[18]

Mendonça TM, Tavares PB, Correia JG, et al. The urea combustion method in the preparation of precursors for high-T_C single phase HgBa₂Ca₂Cu₃O_8+δ superconductors. Physica C 2011, 471: 1643–1646.

DOI Google Scholar

[19]

Isawa K, Tokiwa-Yamamoto A, Itoh M, et al. The effect of Pb doping in HgBa₂Ca₂Cu₃O_8+δ superconductor. Physica C 1993, 217: 11–15.

DOI Google Scholar

[20]

Kirschner I, Laiho R, Lukács P, et al. Effect of preparation on Hg–Ba–Ca–Cu–O superconductors. Z Phys B Con Mat 1996, 99: 501–506.

DOI Google Scholar

[21]

Sin A, Odier P, Weiss F, et al. Synthesis of (Hg,Re-1223) by sol–gel technique. Physica C 2000, 341–348: 2459–2460.

DOI Google Scholar

[22]

Antipov EV, Loureiro SM, Chaillout C, et al. The synthesis and characterization of the HgBa₂Ca₂Cu₃O_8+δ and HgBa₂Ca₃Cu₄O_10+δ phases. Physica C 1993, 215: 1–10.

DOI Google Scholar

[23]

Lin QM, He ZH, Sun YY, et al. Precursor effects on HgBa₂Ca₂Cu₃O₈ formation under high pressure. Physica C 1995, 254: 207–212.

DOI Google Scholar

[24]

Loureiro SM, Stott C, Philip L, et al. The importance of the precursor in high-pressure synthesis of Hg-based superconductors. Physica C 1996, 272: 94–100.

DOI Google Scholar

[25]

Kareiva A, Barkauskas J, Mathur S. Oxygen content and superconducting properties of Hg-based superconductors synthesized by sol–gel method. J Phys Chem Solids 2000, 61: 789–797.

DOI Google Scholar

[26]

Bryntse I, Kareiva A. Superconductivity in HgBa₂Ca₂Cu₃O_8+δ synthesized by different methods. Mater Res Bull 1995, 30: 1207–1216.

DOI Google Scholar

[27]

Przybylski K, Brylewski T. Synthesis of high-T_c (Bi,Pb)–Sr–Ca–Cu–O and Y–Ba–Cu–O superconductors by sol–gel technique. In Proceedings of Join Europe–USA Conferences on Superconductivity ICMAS-92, 1992: 67–72.

Google Scholar

[28]

Brylewski T, Przybylski K. Physicochemical properties of high-T_c (Bi,Pb)–Sr–Ca–Cu–O and Y–Ba–Cu–O superconductors prepared by sol–gel technique. Appl Supercond 1993, 1: 737–744.

DOI Google Scholar

[29]

Sin A, Cunha AG, Calleja A, et al. Influence of precursor oxygen stoichiometry on the formation of Hg, Re-1223 superconductors. Supercond Sci Technol 1999, 12: 120–127.

DOI Google Scholar

[30]

Morawski A, Łada T, Pachla W, et al. Crystal growth of YBa₂Cu₄O₈ superconducting single crystals under high oxygen pressure. In Proceedings of Join Europe–USA Conferences on Superconductivity ICMAS-91, 1991: 361–366.

Google Scholar

[31]

Przybylski K. Physicochemical properties of high-T_c materials—preparation and characterization of Tl–Ba–Ca–Cu–O and Hg–Ba–Ca–Cu–O superconducting thick and thin films. In: Textbook of the 4th International Summer School on High Temperature Superconductivity. Vajda I, Szalay A, Porjesz T, et al. Eds. Eger, Hungary, 1998: 33–61.

[32]

Morawski A, Łada T, Paszewin A, et al. High gas pressure for HTS single crystals and thin layer technology. Supercond Sci Technol 1998, 11: 193–199.

DOI Google Scholar

[33]

Nazzal AI, Lee VY, Engler EM, et al. New procedure for determination of [Cu–O]^+p charge and oxygen content in high T_c copper oxide. Physica C 1988, 153–155: 1367–1368.

DOI Google Scholar

[34]

Bean CP. Magnetization of hard superconductors. Phys Rev Lett 1962, 8: 250.

DOI Google Scholar

[35]

Kakihana M. Invited review “sol–gel” preparation of high temperature superconducting oxides. J Sol–Gel Sci Technol 1996, 6: 7–55.

DOI Google Scholar

[36]

Sillèn LG, Martell AE. Stability constants of metal-ion complexes. Specical Publication No. 25. Chemical Society, London, 1971.

[37]

Day RA Jr., Underwood AL. Quantitative Analysis, Laboratory Manual, 2nd edn. Englewood Cliffs, New Jersey, USA: Prentice-Hall, Inc., 1967.

[38]

Van der Biest O, Kwarciak J, Dierickx D, et al. Ceramic superconductors synthesized by sol–gel methods. Physica C 1991, 190: 119–121.

DOI Google Scholar

[39]

Ringbom A. Complexation in Analytical Chemistry: A Guide for the Critical Selection of Analytical Methods Based on Complexation Reactions. New York: Interscience, 1963.

[40]

Whiter JD, Roth RS. Phase Diagrams for High-T_c Superconductors. Westerville, Ohio, USA: Amer Ceramic Society, 1991.

[41]

Rui Y, Ji HL, Shao HM, et al. Characterization of Hg–Ba–Ca–Cu–O 1223 superconductor. Physica C 1994, 231: 243–248.

DOI Google Scholar

[42]

Martin K, McCarthy G. JCPDS-International Center for Diffraction Data, No. 44-1481.

[43]

Cantoni C, Schilling A, Nissen HU, et al. Characterisation of superconducting Hg–Ba–Ca–Cu–oxides: Structural and physical aspects. Physica C 1993, 215: 11–18.

DOI Google Scholar

[44]

Kellner K, Przybylski K, Gritzner G. Microstructure and phase composition of Hg-1223 bulk phase superconductors. Physica C 1998, 307: 99–104.

DOI Google Scholar

[45]

Przybylski K, Brylewski T, Morawski A, et al. Ba₂Ca₂Cu₃O_x precursor effects on synthesis of (Hg,Pb)Ba₂Ca₂Cu₃O_8+δ superconductor. J Therm Anal Calorim 2001, 65: 391–398.

DOI Google Scholar

[46]

Armstrong

, David

WIF

, Gameson

, et al. Crystal structure of HgBa₂Ca₂Cu₃O_8+δ at high pressure (to 8.5 GPa) determined by powder neutron diffraction. Phys Rev B 1995, 52: 15551-15557.10.1103/PhysRevB.52.15551

DOI Google Scholar

[47]

Abu-Aljarayesh I, Hamam YA, Said MR. Magnetization study of HgBa₂Ca₂Cu₃O_8+δ high-temperature superconductors. Supercond Sci Technol 1997, 10: 290–297.

DOI Google Scholar

About this article

Publication history

Acknowledgements

Rights and permissions

Publication history

Received: 18 August 2015

Revised: 22 March 2016

Accepted: 29 March 2016

Published: 29 June 2016

Issue date: September 2016

Copyright

Acknowledgements

The authors would like to express their gratitude to Mrs. B. Trybalska from the Faculty of Materials Science and Ceramics, AGH University of Science and Technology, Krakow, Poland, for her assistance in SEM–EDX observations.

Rights and permissions

Open Access The articles published in this journal are distributed under the terms of the Creative Commons Attribution 4.0 International License (http://creativecommons. org/licenses/by/4.0/), which permits unrestricted use, distribution, and reproduction in any medium, provided you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons license, and indicate if changes were made.