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Title: New high temperature furnace for structure refinement by powder diffraction in controlled atmospheres using synchrotron radiation

Abstract

A low thermal gradient furnace design is described which utilizes Debye{endash}Scherrer geometry for performing high temperature x-ray powder diffraction with synchrotron radiation at medium and high energies (35{endash}100 keV). The furnace has a maximum operating temperature of 1800 K with a variety of atmospheres including oxidizing, inert, and reducing. The capability for sample rotation, to ensure powder averaging, has been built into the design without compromising thermal stability or atmosphere control. The ability to perform high-resolution Rietveld refinement on data obtained at high temperatures has been demonstrated, and data collected on standard Al{sub 2}O{sub 3} powder is presented. Time-resolved data on the orthorhombic to rhombohedral solid state phase transformation of SrCO{sub 3} is demonstrated using image plates. Rietveld refinable spectra, collected in as little as 8 s, opens the possibility of performing time-resolved structural refinements of phase transformations. {copyright} {ital 1999 American Institute of Physics.}

Authors:
; ;  [1];  [2]; ;  [3];  [4]
  1. Ames Laboratory, U.S. Department of Energy, and Department of Materials Science and Engineering, Iowa State University, Ames, Iowa 50011-3020 (United States)
  2. Cornell High Energy Synchrotron Source (CHESS), Cornell University, Ithaca, New York 14853 (United States)
  3. Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States)
  4. Ames Laboratory, U.S. Department of Energy, and Department of Physics and Astronomy, Iowa State University, Ames, Iowa 50011-3020 (United States)
Publication Date:
OSTI Identifier:
698870
Resource Type:
Journal Article
Journal Name:
Review of Scientific Instruments
Additional Journal Information:
Journal Volume: 70; Journal Issue: 9; Other Information: PBD: Sep 1999
Country of Publication:
United States
Language:
English
Subject:
42 ENGINEERING NOT INCLUDED IN OTHER CATEGORIES; X-RAY DIFFRACTOMETERS; TEMPERATURE CONTROL; STRONTIUM COMPOUNDS; CRYSTAL STRUCTURE; FURNACES; DESIGN; SYNCHROTRON RADIATION; POWDERS; X-RAY DIFFRACTION; GEOMETRY; TEMPERATURE GRADIENTS; STABILITY; OPERATION; TEMPERATURE RANGE 1000-4000 K; CRYSTAL-PHASE TRANSFORMATIONS; ALUMINIUM OXIDES

Citation Formats

Margulies, L., Kramer, M.J., McCallum, R.W., Kycia, S., Haeffner, D.R., Lang, J.C., and Goldman, A.I. New high temperature furnace for structure refinement by powder diffraction in controlled atmospheres using synchrotron radiation. United States: N. p., 1999. Web. doi:10.1063/1.1149948.
Margulies, L., Kramer, M.J., McCallum, R.W., Kycia, S., Haeffner, D.R., Lang, J.C., & Goldman, A.I. New high temperature furnace for structure refinement by powder diffraction in controlled atmospheres using synchrotron radiation. United States. doi:10.1063/1.1149948.
Margulies, L., Kramer, M.J., McCallum, R.W., Kycia, S., Haeffner, D.R., Lang, J.C., and Goldman, A.I. Wed . "New high temperature furnace for structure refinement by powder diffraction in controlled atmospheres using synchrotron radiation". United States. doi:10.1063/1.1149948.
@article{osti_698870,
title = {New high temperature furnace for structure refinement by powder diffraction in controlled atmospheres using synchrotron radiation},
author = {Margulies, L. and Kramer, M.J. and McCallum, R.W. and Kycia, S. and Haeffner, D.R. and Lang, J.C. and Goldman, A.I.},
abstractNote = {A low thermal gradient furnace design is described which utilizes Debye{endash}Scherrer geometry for performing high temperature x-ray powder diffraction with synchrotron radiation at medium and high energies (35{endash}100 keV). The furnace has a maximum operating temperature of 1800 K with a variety of atmospheres including oxidizing, inert, and reducing. The capability for sample rotation, to ensure powder averaging, has been built into the design without compromising thermal stability or atmosphere control. The ability to perform high-resolution Rietveld refinement on data obtained at high temperatures has been demonstrated, and data collected on standard Al{sub 2}O{sub 3} powder is presented. Time-resolved data on the orthorhombic to rhombohedral solid state phase transformation of SrCO{sub 3} is demonstrated using image plates. Rietveld refinable spectra, collected in as little as 8 s, opens the possibility of performing time-resolved structural refinements of phase transformations. {copyright} {ital 1999 American Institute of Physics.}},
doi = {10.1063/1.1149948},
journal = {Review of Scientific Instruments},
number = 9,
volume = 70,
place = {United States},
year = {1999},
month = {9}
}