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Particle and phase thicknesses from XPS analysis of supported bimetallic catalysts: Calcined Co-Rh/Nb{sub 2}O{sub 5}

Journal Article · · Journal of Catalysis
 [1]; ;  [2]
  1. Univ. of Washington, Seattle, WA (United States)
  2. Univ. of Washington, Seattle, WA (United States); and others

The surface structure and elemental composition of a series of calcined Co-Rh/Nb{sub 2}O{sub 5} bimetallic catalysts have been investigated using X-ray photoelectron spectroscopy (XPS) and temperature-programmed reduction (TPR). New formulae for the quantitative analysis of XPS intensities for supported bimetallic catalysts involving up to three separate, layered phases on spherical support particles are used for the first time. These apply an average take-off angle for photoelectrons from spherical particles whose radii are large compared to the electron attenuation length. Calcined monometallic Co/Nb{sub 2}O{sub 5} and Rh/Nb{sub 2}O{sub 5}, and four calcined bimetallic Co-Rh/Nb{sub 2}O{sub 5} catalysts with similar Co loadings ({approx} 1.9 wt%) and variable Rh loadings (0.3 to 2.3 wt%) were examined. Reference spectra for pure CoNb{sub 2}O{sub 6} (columbite) are also presented here for the first time. The catalysts were prepared by incipient wetness impregnation and calcined at 673 K to generate the oxide precursors. The XPS lineshapes and the Co (2p) spin-orbit splitting indicated the presence of two Co species, Co{sub 3}O{sub 4} and CO{sup +2}, on all calcined Co-containing catalysts. The measured XPS Co/Nb and Rh/Nb atomic ratios for the catalysts were factors of 1.5-2 and 2-4.5, respectively, greater than the bulk atomic ratios, showing that both Co and Rh oxides were surface-enriched. The measured XPS peak intensities were compared to the values predicted from several different structural models of the oxide particles.

OSTI ID:
525938
Journal Information:
Journal of Catalysis, Journal Name: Journal of Catalysis Journal Issue: 1 Vol. 152; ISSN 0021-9517; ISSN JCTLA5
Country of Publication:
United States
Language:
English

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