Ln. Wang et al., SYNTHESIS OF NANOPHASE OXALATE PRECURSORS OF YBACUO SUPERCONDUCTOR BYCOPRECIPITATION IN MICROEMULSIONS, Journal of materials chemistry, 5(2), 1995, pp. 309-314
A microemulsion has been studied as a reaction medium to control the c
oprecipitation of oxalate precursors of the superconducting YBa2Cu3O7-
delta ceramics. The oxalate coprecipitation of Y, Ba and Cu from nitra
te solution was studied on basis of computer modelling of equilibrium
systems. The optimum operating conditions, especially the pH range and
concentrations of Y/Ba/Cu/C2O42-, have been estimated. Oxalate coprec
ipitation in stoichiometry of Y:Ba:Cu=1:2:3 is obtained in a pH range
3-4. Phase diagrams of several multicomponent systems: hydrocarbon-aer
osol OT(surfactant)-water, in the absence and presence of nitric/oxali
c acids and nitrates, have been systematically investigated. Among thr
ee hydrocarbons tested, heptane has been found most suitable for the c
oprecipitation of Y, Ba and Cu oxalate. Different stability regions of
microemulsions have been determined. The chemical and morphological p
roperties of the oxalate powders obtained from microemulsions have bee
n examined by ICP, TG, XRD, BET surface area and SEM. These precursors
are nanophase powders with high homogeneity, low crystallinity and ex
act stoichiometry. The average size of the dispersed particles is 50-7
0 nm, while the mean diameter of their agglomerates is around 300 nm.
The best sintered bulk sample has T-c(R=0) at 92 K.