Temperature-programmed reduction (TPR) was performed to investigate the reducibility of the NiO/YSZ composite that is related to the anode of solid oxide fuel cells (SOFCs). The TPR profiles were found to be affected by preparation method, composition and pretreatment conditions. The calcination temperature strongly affected the reduction behavior; the TPR profile of the sample calcined at 1723 K shows a high temperature reduction peak that was not found in the TPR profile of the sample calcined at 1473 K. Such a difference in the TPR profiles can be attributed to the presence of distinct states of NiO species, which are due to the difference of interactions between NiO and YSZ. Five distinct states of NiO species are shown to be present in the NiO/YSZ composite. (C) 2002 Elsevier Science B.V. All rights reserved.