Redox aging above 1000 degrees C of initially high-surface-area (of or
der 100 m(2)/g) cerium-rich ceria-zirconia mixed oxides containing a f
ew wt% Pd results in the loss of most of the surface area and concomit
ant encapsulation of a substantial fraction of the Pd. The encapsulate
d Pd exists in the form of metallic particles on the order of 10 nm in
diameter held under a large (as much as 3.6 GPa) compressive stress b
y the mixed oxide. This stress, evidently arising from changes in latt
ice parameter of the mixed oxide, induced by aging, produces a volume
contraction of Pd, which appears as a shift of Pd-peak positions in XR
D measurements. Subsequent reduction and reoxidation of the mixed oxid
e in turn relieves and restores the stress on the Pd particles, which
remain metallic throughout, demonstrating that this portion of the Pd
is effectively lost for catalytic purposes.