Abrupt and reversible changes in the oxygen content and the electrical
conductivity have been detected at similar to 500 degrees C in the an
ion-deficient perovskite LaCu(1-x)Ni(x)O(2.5+)delta, which was synthet
ized as part of this study. These changes accompany a transition from
a metallic to a semiconducting behavior. The changes were found by x-r
ay diffraction, differential thermal analysis, thermogravimetry, and m
easurements of the electrical conductivity. The anomalies observed her
e are shown to be accompanied by a structural phase transition and are
linked with a sharp change in the Cu3+/Cu2+ cation ratio in the low-
and high-temperature phases.