The formation of insulating phases at the interface between cathode and ele
ctrolyte materials during solid oxide fuel cell (SOFC) operation leads to d
eleterious effects on SOFC properties. We report in situ impedance spectros
copy measurements of the degradation process of porous La0.65Sr0.35MnO3/Zr0
.84Y0.16O1.92 electrodes submitted to annealing temperatures above normal S
OFC operating temperature, which is around 1173 K, simulating longterm SOFC
operation. To measure the remaining effects after high-temperature anneali
ng, impedance diagrams were plotted during the entire heating process up to
the annealing temperatures, and during the complete cooling process. These
diagrams were also plotted during the aging periods to follow the overall
degradation. It was possible to detect and quantify electrical and electroc
hemical degradations, which are related to the formation of insulating phas
es at the electrode/electrolyte interface. Samples were annealed for about
200 h in air at temperatures between 1373 and 1673 K. Scanning electron mic
roscopy and energy-dispersive X-ray spectrometry were also used to detect m
icrostructural changes at the electrode.