Nickel was impregnated into a porous scandia-stabilised zirconia scaffold through 12 impregnation cycles. The impregnated electrodes contained approximately 40 wt% of nickel. Continuous van der Pauw measurement was carried out when the electrode was aged at 650 oC, 800 oC and 950 oC in an atmosphere with 5 vol% hydrogen and 95 vol% nitrogen, at open circuit. A fall in sheet conductivity was found in the electrode during ageing within 1000 min. The conductivity fall was attributed to nickel microstructural evolution during ageing. Electrochemical impedance spectra were collected at a constant time intervals during isothermal annealing at 650 oC, 800 oC and 950 oC for the impregnated electrode. Four resistance contributions were decoupled by equivalent circuit fitting, i.e. the ohmic resistance, the oxygen transfer resistance and the anodic reaction resistance, and the gas diffusion resistance. The increase in both the ohmic resistance and the polarisation resistances with time revealed the isothermal degradation brought about a diminishing active anode area. A more pronounced decrease in anodic polarisation resistance suggested a reduction in triple phase boundary (TPB) density. Secondary electron images of electrodes before and after ageing showed an increase in nickel particle size and a decrease in the number of particles, providing microstructural evidence of nickel coarsening. Nickel coarsening was identified as the main mechanism of degradation for the electrode in wet hydrogen as it caused a reduction in both TPB sites and percolating nickel paths. Combining time-dependent electrochemical performance with post-mortem electrode microstructure clarifies the physical processes behind the degradation quantified by increasing area specific resistances.
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