Synthesis, microstructural evolution and the role of substantial addition of PbO during the final processing of (Bi,Pb)-2223 superconductors

The evolution of the phase formation and microstructure in (Bi,Pb)-Sr-Ca-Cu-O (BPSCCO) superconducting materials have been studied through a two-cycle annealing process by X-ray diffraction and SEM observations. Samples were Pb-doped (part 0.4 of Bi substituted by Pb) during the first thermal cycle. Yet, the synthesizing efficiency of the (Bi,Pb)-2223 phase was found to be greatly re-enhanced during the second thermal cycle by a second and substantial addition of up to 20% excess of PbO in weight. No significant increase of secondary phases was observed. Pb addition was shown to be more effective at the end of a multi-step thermal cycle. Therefore the lack of Pb that arise in BPSCCO system after some heat treatment duration is shown to be one of the most important rate-limiting (Bi,Pb)-2223 transformation. The second sintering duration at 835 degreesC was optimized with respect to the weight percentage of PbO in excess. The present work attempts also to point out the complex mechanisms of the (Bi,Pb)-2223 formation reactions. Some intermediate phases are identified and the liquid phase is suggested to derive from a partial decomposition of the (Bi,Pb)-2212 phase. This decomposition is highly sensitive to Pb addition. (C) 2001 Elsevier Science B.V. All rights reserved.