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°C 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.