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Performance of a new furnace for high‐resolution synchrotron powder diffraction up to 1900 K: application to determine electron density distribution of the cubic CaTiO 3 perovskite at 1674 K
Author(s) -
Yashima Masatomo,
Tanaka Masahiko
Publication year - 2004
Publication title -
journal of applied crystallography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.429
H-Index - 162
ISSN - 1600-5767
DOI - 10.1107/s002188980401698x
Subject(s) - materials science , perovskite (structure) , synchrotron , rietveld refinement , beamline , powder diffraction , diffraction , analytical chemistry (journal) , synchrotron radiation , crystal structure , ionic bonding , crystallography , chemistry , ion , optics , beam (structure) , physics , chromatography , organic chemistry
Accurate crystal structure analysis at high temperatures is an important challenge in science and technology. A new electric furnace for the measurement of high‐resolution (δ d / d = 0.03%) synchrotron radiation powder diffraction profiles from materials at high temperatures (up to 1900 K in air) has been designed and fabricated. This furnace consists of a ceramic refractory with MoSi 2 heaters, an aluminium body cooled by flowing water, and a sample stage with a spinner and a controller for sample‐height adjustment. In situ synchrotron powder diffraction measurement for a calcium titanate perovskite specimen at 1674 K has been performed using the furnace at beamline 3A of the Photon Factory. The electron density distribution of the cubic perovskite at 1674 K was successfully obtained using a combination of Rietveld refinement, the maximum‐entropy method (MEM) and MEM‐based pattern‐fitting techniques. The Ti atoms exhibit covalent bonding with the O atoms in the cubic CaTiO 3 perovskite at this temperature, while the Ca atoms are ionic. These results indicate that the new furnace yields high‐quality data for accurate crystal structure analysis.