V. Primo et al., FAST SYNTHESIS OF SINGLE-PHASED 110-K BISMUTH SUPERCONDUCTOR BY FREEZE-DRYING OF ACETIC PRECURSORS - KINETIC ROLE OF CALCIUM AND COPPER OXIDES, Solid state ionics, 63-5, 1993, pp. 872-882
Although the usefulness of solution procedures to improve the synthesi
s of bismuth HTSC has been argued, an adequate control of the procedur
al variables has allowed us to isolate the 110 K phase as the only sup
erconducting phase after such a short sintering time as 22 h. The prec
ursors used have been freeze-dried powders resulting from acetic solut
ions containing excess Ca and Cu. TGA-DTA and XRD experiments have bee
n performed to follow the subsequent solid-state reaction processes. T
he initial formation of a mixed bismuth-lead oxoacetate, as intermedia
te to (Bi1-yPby)2Pby)2CuO4, and the presence of an excess of Ca2CuO3 i
n the last reaction step are two of the main factors driving the fast
synthesis of the 110 K phase.