The cerium species have been characterized during the temperature-programmed reduction (TPR) process under H
2 atmosphere by means of the X-ray absorption fine structure (XAFS) spectroscopy and the X-ray diffraction (XRD) method. The in-situ XAFS measurements revealed that the CeO
2 species was finally reduced to Ce
2O
3 at 900 ºC with an intermediate state generated in the temperature rage of 550–750 ºC. The absorption edge shift of the X-ray absorption near edge structure (XANES) spectra indicated that the non-stoichiometric compound was formed as the intermediate species, and the estimated composition was CeO
1.65. The in-situ XRD measurements during the TPR process showed the shift of the diffraction lines of CeO
2 above 400 ºC, indicating the formation of the non-stoichiometric intermediate. The quantitative analysis of the lattice parameter demonstrated that the crystal plane spacing for the (111) plane of the non-stoichiometric intermediate was expanded by about 0.03 Å than the initial CeO
2 phase.
View full abstract