Abstract
Calcium plumbate Ca2PbO4 was prepared by sol–gel methods (Pechini complex route with two varieties and water soluble polymer method) and by solid state reaction. The sol–gel prepared samples contained calcium plumbate as the only one phase as early as after 2 h annealing at 800 °C. Phase composition was detected by XRD measurement and by Raman spectroscopy. The next annealing at 800 °C for 24 h induced weak Pb losses displayed by present CaO (according to phase equilibrium) and confirmed by XRF measurement. The Pb losses were smaller for the sol–gel prepared samples probably due to earlier formation of Ca2PbO4. Microstructure and grain size were also established. Sol–gel prepared samples had regularly distributed grains with a small distribution interval with median value in order of 1 μm. Differences in microstructure of solid state and sol–gel samples are presented on SEM micrographs.
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References
Grivel JC, Flukiger R (1998) Formation mechanism of the Pb free Bi2Sr2Ca2Cu3O10 phase. Supercond Sci Technol 11(3):288–298. doi:10.1088/0953-2048/11/3/007
Li MY, Han Z (2007) The effect of lead-rich phases on the microstructure and properties of (Bi, Pb)-2223/Ag tapes. Supercond Sci Technol 20(8):843–850. doi:10.1088/0953-2048/20/8/021
Troemel M (1965) Zur Struktur der Verbindungen vom Sr2PbO4-Typ. Naturwissenschaften 52:492–493. doi:10.1007/BF00646570
Teichert A, Mullerbuschbaum H (1992) On the crystal structure of Ca2PbO4. Z Anorg Allg Chem 607(1):128–130. doi:10.1002/zaac.19926070122
Kitaguchi H, Takada J, Oda K, Miura Y (1990) Equilibrium phase diagram for the system PbO–CaO–CuO. J Mater Res 5(5):929–931. doi:10.1557/JMR.1990.0929
Jeremie A, Grasso G, Flukiger R (1997) Synthesis and characterization of high temperature superconductors system Bi–Pb–Sr–Ca–Cu–O. J Therm Anal 48(3):635–645. doi:10.1007/BF01979509
Martini PL, Bianchini A (1969) Formation of calcium plumbate—kinetics and mechanism of reaction. J Appl Chem Ussr 19(5):147–152
Kakihana M (1996) ‘‘Sol–Gel’’ preparation of high temperature superconducting oxides. J Sol–Gel Sci Technol 6(1):7–55. doi:10.1007/BF00402588
Sykorova D, Smrckova O, Rubesova K, Vasek P (2007) Comparative study of Bi-2223/Ag superconductors derived from particles size of starting materials. Int J Mod Phys B 21(18–19):3246–3249. doi:10.1142/S0217979207044299
Pechini MP (1967) US Patent 3,330,697
Sotelo A, Delafuente GF, Lera F, Beltran D, Sapina F, Ibanez R, Beltran A, Bermejo MR (1993) Novel polymer solution synthesis of the 110 K superconducting phase in the bismuth system. Chem Mater 5(6):851–856. doi:10.1021/cm00030a022
Kakihana M, Okubo T, Arima M, Nakamura Y, Yashima M, Yoshimura M (1998) Polymerized complex route to the synthesis of pure SrTiO3 at reduced temperatures: implication for formation of Sr–Ti heterometallic citric acid complex. J Sol–Gel Sci Technol 12(2):95–109. doi:10.1023/A:1008613312025
Rubesova K, Sykorova D (2006) Preparation of strontium vanadate Sr3V2O8 as additive to Bi-based superconductors. Adv Sci Technol 47:49–54
Werner P-E, Eriksson L, Westdahl M (1985) TREOR, a semi-exhaustive trial-and-error powder indexing program for all symmetries. J Appl Cryst 18(5):367–370. doi:10.1107/S0021889885010512
Braileanu A, Zaharescu M, Crisan D, Segal E (1995) Thermoanalytical study of compound formation in the Bi2O3–PbO–CaO system. Thermochim Acta 269–270:553–565. doi:10.1016/0040-6031(95)02565-0
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This work was financially supported by MSMT CR as the project No. 604613730.
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Rubešová, K., Sýkorová, D. Preparation of calcium plumbate via different route. J Sol-Gel Sci Technol 49, 228–232 (2009). https://doi.org/10.1007/s10971-008-1848-3
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DOI: https://doi.org/10.1007/s10971-008-1848-3