Js. Luo et al., COMPOSITION AND MICROSTRUCTURAL EVOLUTION OF NONSUPERCONDUCTING PHASES IN SILVER-CLAD (BI,PB)2SR2CA2CU3OX COMPOSITE CONDUCTORS, Journal of materials research, 9(12), 1994, pp. 3059-3067
The composition and microstructural evolution of nonsuperconducting ph
ases during the course of formation of (Bi,Pb)2Sr2Ca2Cu3Ox (Bi-2223) i
n a silver sheath have been investigated by x-ray diffraction (XRD) an
alysis, scanning electron microscopy (SEM), energy dispersive x-ray sp
ectroscopy (EDX), and digital image analysis. Wire samples fabricated
by the oxide-powder-in-tube technique were heat-treated under a variet
y of conditions (time, temperature, and oxygen pressure). Backscattere
d images taken on polished but unetched transverse cross sections were
subjected to computerized image processing, which allowed determinati
on of the stoichiometry and quantification of microstructural characte
ristics (such as area fraction, size distribution, position, and orien
tation) of each nonsuperconducting particle. The dominant nonsupercond
ucting phases observed by SEM/EDX were CuO, (Ca, Sr)2CuO3 (2/1), and (
Ca, Sr)14Cu24O41 (14/24) in amounts that varied depending on the annea
ling temperature, time, and oxygen partial pressure. Time evolution st
udies performed at 825-degrees-C in 0.075 atm O2 showed that the area
fraction of 2/1 decreased with reaction time, while that for 14/24 inc
reased. In all cases, a substantial amount (> 10% area fraction) of no
nsuperconducting phases was detected even after all the Bi2Sr2CaCu2Oy
(Bi-2212) in the as-rolled composite conductor was fully converted to
Bi-2223, as determined by XRD. High aspect ratio nonsuperconducting pa
rticles were initially randomly oriented in the composite conductor co
re but gradually aligned parallel to the silver/(Bi,Pb)-Sr-Ca-Cu-O int
erface after extended annealing. They tended to segregate and exhibite
d a much broader size distribution when processing was carried out at
temperatures and oxygen partial pressures on the high end of the norma
l processing range, most likely as a result of the occurrence of parti
al melting in the system.