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Determining metal ion distributions using resonant scattering at very high-energy K-edges: Bi/Pb in Pb{sub 5}Bi{sub 6}Se{sub 14}

Abstract

Powder diffraction data collected at {proportional_to} 86 keV, and just below both the Pb and the Bi K-edges, on an imaging plate detector using synchrotron radiation from the Advanced Photon Source have been used to examine the Pb/Bi distribution over the 11 crystallographically distinct sites in Pb{sub 5}Bi{sub 6}Se{sub 14} [space group P2{sub 1}/m, a=16.0096(2) Aa, b=4.20148(4) Aa, c=21.5689(3) Aa and {beta}=97.537(1){sup 0}]. The scattering factors needed for the analyses were determined both by Kramers- Kronig transformation of absorption spectra and by analyses of diffraction patterns from reference compounds. Even with the relatively low scattering contrast that is available at the K-edges, it was possible to determine the Pb/Bi distribution and probe the presence of cation site vacancies in the material. The current results indicate that resonant scattering measurements at high-energy K-edges are a viable, and perhaps preferable, route to site occupancies when absorption from the sample or sample environment/container is a major barrier to the acquisition of high-quality resonant scattering data at lower-energy edges.
Authors:
Yuegang, Zhang; Lee, P L; Shastri, S D; Deming, Shu; [1]  Wilkinson, A P; [2]  Duck-Young, Chung; Kanatzidis, M G [3] 
  1. Argonne National Lab., IL (United States). XOR, Advanced Photon Source
  2. Georgia Inst. of Tech., Atlanta (United States). School of Chemistry and Biochemistry
  3. Michigan State Univ., East Lansing (United States). Dept. of Chemistry
Publication Date:
Jun 01, 2005
Product Type:
Journal Article
Resource Relation:
Journal Name: Journal of Applied Crystallography; Journal Volume: 38; Journal Issue: 3; Other Information: PBD: Jun 2005
Subject:
36 MATERIALS SCIENCE; ABSORPTION SPECTRA; BISMUTH IONS; BISMUTH SELENIDES; CRYSTAL LATTICES; DEBYE-SCHERRER METHOD; ENERGY SPECTRA; EXPERIMENTAL DATA; ION DENSITY; KEV RANGE 10-100; LEAD IONS; LEAD SELENIDES; RESONANCE SCATTERING; VACANCIES; X-RAY DIFFRACTION; X-RAY SPECTRA
OSTI ID:
20623331
Country of Origin:
Denmark
Language:
English
Other Identifying Numbers:
Journal ID: ISSN 0021-8898; JACGAR; TRN: DK05FA064066410
Availability:
Available from: http://dx.doi.org/10.1107/S0021889805005686;INIS
Submitting Site:
DKN
Size:
page(s) 433-441
Announcement Date:
Aug 28, 2005

Citation Formats

Yuegang, Zhang, Lee, P L, Shastri, S D, Deming, Shu, Wilkinson, A P, Duck-Young, Chung, and Kanatzidis, M G. Determining metal ion distributions using resonant scattering at very high-energy K-edges: Bi/Pb in Pb{sub 5}Bi{sub 6}Se{sub 14}. Denmark: N. p., 2005. Web. doi:10.1107/S0021889805005686.
Yuegang, Zhang, Lee, P L, Shastri, S D, Deming, Shu, Wilkinson, A P, Duck-Young, Chung, & Kanatzidis, M G. Determining metal ion distributions using resonant scattering at very high-energy K-edges: Bi/Pb in Pb{sub 5}Bi{sub 6}Se{sub 14}. Denmark. https://doi.org/10.1107/S0021889805005686
Yuegang, Zhang, Lee, P L, Shastri, S D, Deming, Shu, Wilkinson, A P, Duck-Young, Chung, and Kanatzidis, M G. 2005. "Determining metal ion distributions using resonant scattering at very high-energy K-edges: Bi/Pb in Pb{sub 5}Bi{sub 6}Se{sub 14}." Denmark. https://doi.org/10.1107/S0021889805005686.
@misc{etde_20623331,
title = {Determining metal ion distributions using resonant scattering at very high-energy K-edges: Bi/Pb in Pb{sub 5}Bi{sub 6}Se{sub 14}}
author = {Yuegang, Zhang, Lee, P L, Shastri, S D, Deming, Shu, Wilkinson, A P, Duck-Young, Chung, and Kanatzidis, M G}
abstractNote = {Powder diffraction data collected at {proportional_to} 86 keV, and just below both the Pb and the Bi K-edges, on an imaging plate detector using synchrotron radiation from the Advanced Photon Source have been used to examine the Pb/Bi distribution over the 11 crystallographically distinct sites in Pb{sub 5}Bi{sub 6}Se{sub 14} [space group P2{sub 1}/m, a=16.0096(2) Aa, b=4.20148(4) Aa, c=21.5689(3) Aa and {beta}=97.537(1){sup 0}]. The scattering factors needed for the analyses were determined both by Kramers- Kronig transformation of absorption spectra and by analyses of diffraction patterns from reference compounds. Even with the relatively low scattering contrast that is available at the K-edges, it was possible to determine the Pb/Bi distribution and probe the presence of cation site vacancies in the material. The current results indicate that resonant scattering measurements at high-energy K-edges are a viable, and perhaps preferable, route to site occupancies when absorption from the sample or sample environment/container is a major barrier to the acquisition of high-quality resonant scattering data at lower-energy edges.}
doi = {10.1107/S0021889805005686}
journal = []
issue = {3}
volume = {38}
journal type = {AC}
place = {Denmark}
year = {2005}
month = {Jun}
}