Neutron powder diffraction study of sulfated zirconia catalysts

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In situ neutron powder diffraction method was used to investigate the crystal structures, phase abundance and thermal stability of sulfated zirconia catalysts prepared by impregnation of hydrous zirconium oxide gels with 0.5 M H{sub 2}SO{sub 4} solutions. The sample studied was precipitated at pH = 10 and dried for 5 h at 493 K, and then calcined at 853 K for 3 h. Diffraction data were collected in the temperature range 295-1273 K in an Ar atmosphere and analyzed using the Rietveld method. Only the metastable tetragonal phase was observed below 673 K. Above this temperature, the sample consisted of ... continued below

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9 p.

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Li, X.; Lager, G.A. & Loong, C.K. July 1, 1997.

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  • Li, X. Univ. of Louisville, KY (United States). Dept of Chemical Engineering
  • Lager, G.A. Univ. of Louisville, KY (United States). Dept. of Geography and Geosciences
  • Loong, C.K. Argonne National Lab. IL (United States)

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Description

In situ neutron powder diffraction method was used to investigate the crystal structures, phase abundance and thermal stability of sulfated zirconia catalysts prepared by impregnation of hydrous zirconium oxide gels with 0.5 M H{sub 2}SO{sub 4} solutions. The sample studied was precipitated at pH = 10 and dried for 5 h at 493 K, and then calcined at 853 K for 3 h. Diffraction data were collected in the temperature range 295-1273 K in an Ar atmosphere and analyzed using the Rietveld method. Only the metastable tetragonal phase was observed below 673 K. Above this temperature, the sample consisted of a mixture of tetragonal (T) and monoclinic (M) phases in the proportions (T:M wt%) 85:15 (1073 K) and 61:39 (1273 K). Surface modification by sulfation was found to retard the onset of the tetragonal-to-monoclinic transformation relative to pure zirconia. The decrease in peak-broadening at the higher temperatures reflects both an increase in crystallite size and a decrease in microstrain.

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9 p.

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INIS; OSTI as DE97054130

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  • International conference on neutron scattering (ICNS), Toronto (Canada), 17-21 Aug 1997

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  • Other: DE97054130
  • Report No.: ANL/IPNS/CP--93088
  • Report No.: CONF-970814--
  • Grant Number: W-31-109-ENG-38
  • Office of Scientific & Technical Information Report Number: 565539
  • Archival Resource Key: ark:/67531/metadc694643

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  • July 1, 1997

Added to The UNT Digital Library

  • Aug. 14, 2015, 8:43 a.m.

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  • Dec. 15, 2015, 11:59 a.m.

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Li, X.; Lager, G.A. & Loong, C.K. Neutron powder diffraction study of sulfated zirconia catalysts, article, July 1, 1997; Illinois. (digital.library.unt.edu/ark:/67531/metadc694643/: accessed September 18, 2018), University of North Texas Libraries, Digital Library, digital.library.unt.edu; crediting UNT Libraries Government Documents Department.