Temperature induced degradation in Solid Oxide Fuel Cell (SOFC) Ni-YSZ anodes was studied using both impedance spectroscopy and three-dimensional tomography via Focused Ion Beam-Scanning Electron Microscopy. A 100 h anneal at 1100 degrees C caused a 90% increase in cell polarization resistance, which correlated with the observed factor of similar to 2 reduction in the electrochemically active three-phase boundary (TPB) density. The TPB decrease was caused by a significant decrease in pore percolation, and a reduction in pore interfacial area due to pores becoming larger and more equiaxed. The anneal caused no measurable change in average Ni particle size; Ni coarsening was apparently highly constrained in these anodes due to the relatively large YSZ volume fraction and low pore volume. (C) 2010 Elsevier B.V. All rights reserved.