Preparation and characterization of superconducting phases in the Bi(Pb)-Sr-Ca-Cu-O system

The superconductive properties in the Bi(Pb)-Sr-Ca-Cu-O system with nominal composition of Bi2−x Pbx Sr2 Ca2 Cu3 Oy (x=0, 0.2, 0.4, and 0.6) and annealed at 860 °C for 240 h were studied using dc resistivity and ac susceptibility measurements. For x=0.2 and 0.4, the bulk zero resistivity temperatures were found to be ∼103 K. For x=0 and 0.6, these temperatures were found to be ∼73–75 K. The ac susceptibility data show enrichment of the volume fraction of the high-Tc phase in compositions with x=0.2 and 0.4. Tc of this phase is constant at 107 K for all values of x. The enhancement of the bulk zero resistivity temperature for x=0.2 and 0.4 is due to the improved intergranular coupling of the high-Tc phase, although the resulting weak-link behavior reflects a low current carrying capacity in these materials. The presence of the low-Tc phase (∼65 K) is still visible in the susceptibility data. For x=0.6, the intergranular coupling of the high-Tc phase is almost destroyed; however, the coupling of the low-Tc phase is better than when x=0. Powder x-ray diffraction and scanning electron microscopy data show the formation of large grains of the calcium plumbate, Ca2PbO4 phase with increasing Pb up to x=0.6. The large grains of the Ca2 PbO4 phase may incorporate other impurity phases within it when x=0.6, cleaning up the remaining grain boundaries, thereby improving the intergranular coupling within this material. Energy dispersive x-ray analysis indicates that some Pb is incorporated into the structure of both superconducting phases.