W0048
In-situ Neutron Diffraction Studies of
SrFeCo0.5Ox Ceramic Membrane under pO2
Gradients. Yaping Li, Evan R. Maxey and James W. Richardson Jr., Intense
Pulsed Neutron Source, Argonne National Laboratory Argonne, IL 60439.
Understanding the performance of multi-phase
SrFeCo0.5Ox (SFC2) membranes operating at elevated
temperature and pO2 gradients relies on accurate determination of
both structural and phase stability of the ceramic membranes. An air-sintered
dense ceramic membrane with composition SFC2 was prepared by solid-state
reactions. In-situ time-of-flight neutron diffraction data were collected
on the membrane with a wall thickness of ~1 mm that was exposed on one side to
air with pO2’ of ~10-0.9 atm, and to
pO2” of reducing atmosphere on the other side under isothermal
condition (~900ºC), and neutron diffraction data were analyzed through
Rietveld refinements. Phase evolution of SFC2 was investigated through changing
the pO2” in the range of ~10-0.9 –
10-17.5 atm. At least a total of six phases were identified in the
diffraction patterns with various pO2 gradients, including
intergrowth 236, perovskite, brownmillerite, rocksalt, and metallic phases (_
and _). Our results revealed that the phase composition of SFC2 is dependent
upon the pO2” on the reducing side, and that the phase
evolution of the SFC2 membrane under pO2 gradients is much more
complex than previously thought; based on static studies with pO2
down to 10-15 atm. The 236 can remain in the SFC2 at
pO2” of ~10-15 atm, and was completely decomposed to
perovskite and rocksalt at pO2” of 10-17 atm,
demonstrating that the stability field of 236 was extended to lower
pO2 region by oxygen transported from the oxidizing side. Perovskite
was stable in entire pO2 gradients, and a small amount of oxygen
vacancy ordered brownmillerite was found at strongly reducing atmosphere.
Metallic phases of _ and _-(Co,Fe) were observed at pO2” of
~10-15 atm from the reduction of rocksalt. The structures of 236 and
rocksalt can be reestablished when pO2” went back to
10-15 atm. It is expected that this complex assemblage of multiple
phases in SFC2 at pO2 gradient has significant impact on the mixed
conducting behavior of SFC2 membranes.