Characterization of structural and surface properties of nanocrystalline TiO2-CeO2 mixed oxides by XRD, XPS, TPR, and TPD

Shingo Watanabe, Xiaoliang Ma, Chunshan Song

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346 Scopus citations


This work focuses on characterizing the structural and surface properties of TiXCe1-X O2 (TiO2-CeO 2) mixed oxides using XRD, XPS, BET, H2-TPR, and NH3-TPD techniques. The TiXCe1-X O2 mixed oxides synthesized by the urea coprecipitation method showed unimodal nanoporous structure with pore sizes increasing from 3.7 nm for X = 0.9 to 5.3 nm for X = 0.1. Concomitant with their higher surface area and pore volume, the mixed oxides were nanocrystalline, about 4.0 nm in crystallite size when X = 0.9, and 4.8-5.4 nm when X = 0.1-0.3, which are significantly smaller than TiO 2 and CeO2 single oxides prepared by the same method (8.1 to 8.4 nm). A dominant anatase phase was detected by XRD when X was 0.9 or higher while a cubic fluorite phase was dominant when X was 0.3 or lower. Lattice parameters were changed by incorporating Ce into TiO2, and Ti into CeO2, respectively. This change indicates distortion of structure and was attributed to reduction of Ti4+ to Ti3+, and Ce4+ to Ce3+. XPS (Ce 3d, Ti 2p, O 1s) and H 2-TPR revealed that the oxidation state of surface cations decreased, and oxygen deficiency of the surface was significantly enhanced by introducing Ce into TiO2, and Ti into CeO2. The structural and surface modification by introducing Ce into TiO2 increased the reducibility of mixed oxides in H2-TPR. NH3-TPD showed that increasing Ti content in TiXCe1-X O2 enhanced surface acidity. Furthermore, H2O and N2 formation from NH 3 was detected by mass spectrometry, which was attributed to the oxidation activity of the TiXCe1-X O2 mixed oxides. The highest NH3 oxidation activity was observed when X = 0.9. The present study clearly established that the structural (crystal phase, crystal size, nanoporosity, pore size) and surface properties (reducibility, oxygen deficiency, acidity, oxidation activity) of the TiXCe 1-X O2 mixed oxides can be tailored by controlling their composition by the urea coprecipitation procedure.

Original languageEnglish (US)
Pages (from-to)14249-14257
Number of pages9
JournalJournal of Physical Chemistry C
Issue number32
StatePublished - Aug 13 2009

All Science Journal Classification (ASJC) codes

  • Electronic, Optical and Magnetic Materials
  • General Energy
  • Physical and Theoretical Chemistry
  • Surfaces, Coatings and Films


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