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Effect of LiF addition on the phase transition of sinterable β-spodumene precursor powders prepared by a sol-gel process

Published online by Cambridge University Press:  31 January 2011

Moo-Chin Wang ,
Nan-Chung Wu ,
Sheng Yang  and
Shaw-Bing Wen
Moo-Chin Wang
Affiliation:
Department of Mechanical Engineering, National Kaohsiung University of Applied Sciences, 415 Chien-Kung Road, Kaohsiung, 80782, Taiwan
Nan-Chung Wu
Affiliation:
Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan, 70101, Taiwan
Sheng Yang
Affiliation:
Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan, 70101, Taiwan
Shaw-Bing Wen
Affiliation:
Department of Resources Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan, 70101, Taiwan
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Abstract

β-Spodumene (Li2O · Al2O · 4SiO2, LAS4) precursor powders were obtained through a sol-gel process using Si(OC2H5)4, Al(OC4H9)3, and LiNO3 as starting materials and LiF as a sintering aid. X-ray diffraction, scanning electron microscopy, scanning transmission electron microscopy with a wavelength dispersive spectrometer, and electron diffraction analysis were utilized to study the phase transition of the β-spodumene glass–ceramics prepared from the gel-derived precursor powders with LiF additive. For the LAS4 precursor powders containing no LiF, the only crystalline phase obtained was β-spodumene. For the pellets containing less than 4.0 wt% LiF and sintered at 1050 °C for 5 h, the crystalline phases were β-spodumene solid solution and β-eucryptite (Li2O · Al2O3 · 2SiO2, LAS2) solid solution. When the LiF content was 5.0 wt% and the sintering process was carried out at 1050 °C for 5 h, the crystalline phases were β-spodumene solid solution, β-eucryptite solid solution (triclinic), and eucryptite [rhombohedral (hex.)]. When the LiF addition attains 3.0 wt%, the fully densified grains are formed, accompanied with an increase in grain size for LiF addition. At the triple junction of grain boundaries a second phase segregates which is identified to be β-spodumene solid solution. In the sintering period of LAS4 precursor powders with LiF additive, the grains converted to β-eucryptite solid solution and β-spodumene solid solution remains at the grain boundaries.

Type
Articles
Information
Journal of Materials Research , Volume 17 , Issue 8 , August 2002 , pp. 1960 - 1968
Copyright
Copyright © Materials Research Society 2002

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