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Structural Properties of β-FeSi2 Bulk Crystal Grown by Horizontal Gradient Freeze Method

Published online by Cambridge University Press:  15 February 2011

H. Kakemoto ,
Y. Tsaic ,
A. C. Beye ,
H. Katsumata ,
S. Sakuragi ,
Y. Makita ,
A. Obaraa ,
N. Kobayashi ,
H. Shibata  and
S. Uekusa
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H. Kakemoto
Affiliation:
Electrotechnical Laboratory, 1-1-4 Umezono, Tsukuba, Ibaraki 305, Japan. Science University of Tokyo, 1-3 Kagurazaka, Shinjuku, Tokyo 162, Japan.
Y. Tsaic
Affiliation:
Union Material, 1640 Oshido-jyodai, Tonemachi, Ibaraki 270-12, Japan.
A. C. Beye
Affiliation:
Electrotechnical Laboratory, 1-1-4 Umezono, Tsukuba, Ibaraki 305, Japan. University Cheikh Anta Diop of Dakar, GPSSM, B.P. 5376, Dakar, Senegal.
H. Katsumata
Affiliation:
Electrotechnical Laboratory, 1-1-4 Umezono, Tsukuba, Ibaraki 305, Japan. Meiji University, 1-1-1 Higashi-mita, Tama, Kawasaki, Kanagawa 214, Japan.
S. Sakuragi
Affiliation:
Union Material, 1640 Oshido-jyodai, Tonemachi, Ibaraki 270-12, Japan.
Y. Makita
Affiliation:
Electrotechnical Laboratory, 1-1-4 Umezono, Tsukuba, Ibaraki 305, Japan.
A. Obaraa
Affiliation:
Electrotechnical Laboratory, 1-1-4 Umezono, Tsukuba, Ibaraki 305, Japan.
N. Kobayashi
Affiliation:
Electrotechnical Laboratory, 1-1-4 Umezono, Tsukuba, Ibaraki 305, Japan.
H. Shibata
Affiliation:
Electrotechnical Laboratory, 1-1-4 Umezono, Tsukuba, Ibaraki 305, Japan.
S. Uekusa
Affiliation:
Meiji University, 1-1-1 Higashi-mita, Tama, Kawasaki, Kanagawa 214, Japan.
T. Tsukamoto
Affiliation:
Science University of Tokyo, 1-3 Kagurazaka, Shinjuku, Tokyo 162, Japan.
T. Tsunoda
Affiliation:
National Institute of Material and Chemical Research, 1-1 Tsukuba-Higashi, Ibaraki 305, Japan.
Y. Imaif
Affiliation:
National Institute of Material and Chemical Research, 1-1 Tsukuba-Higashi, Ibaraki 305, Japan.
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Abstract

We report on the synthesis of β-FeSi2 bulk materials using Horizontal Gradient Freeze (HGF) method. Chunk and powder FeSi2 or high-purity Fe (4N) and Si (9N) were used as starting materials. Three values (1:2, 2:5 and 1:3) of the Fe:Si ratio were selected in the very narrow α and β ranges of the equilibrium phase diagram. Samples were melted between 1300°C and 1500°C in high purity graphite crucibles covered with boron nitride. After cooling, the samples were kept at 800°C and 900°C during 66 to 100 hours, leading to transformation from α to β phase. Cooling rate and annealing time were taken as the two main parameters to optimize the growth conditions. Principal structural characterization was made by X-ray diffraction (XRD). Correlation with stoichiometry was achieved using the results of Rutherford Backscattering Spectroscopy (RBS) and Electron Probe X-Ray Micro Analysis (EPXMA). The samples obtained from 1:2 ratio exhibited mainly β phase while the 2:5 ratio specimens revealed almost α phase structure. The samples prepared with 1:3 ratio was found as a mixture of α and β phases under Si-rich conditions.

Type
Research Article
Information
MRS Online Proceedings Library (OPL) , Volume 402: Symposium H – Silicide Thin Films-Fabrication, Properties and Applications , 1995 , 331
Copyright
Copyright © Materials Research Society 1996

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