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Title: Formation of {alpha}-eucryptite, LiAlSiO{sub 4}: An in-situ synchrotron X-ray powder diffraction study of a high temperature hydrothermal synthesis

Abstract

Hydrothermal conversion of zeolite Li-A(BW), LiAlSiO{sub 4}{center_dot}H{sub 2}O, into {alpha}-eucryptite, LiAlSiO{sub 4}, occurs at temperatures above 350 C. The authors report here the first in-situ study of a high-temperature hydrothermal synthesis using time-resolved power diffraction. The hydrothermal syntheses were performed in stainless steel capillaries. To maintain hydrothermal conditions, a hydraulic pressure of 2--300 atm was applied. Synchrotron X-ray radiation with energies of 35--40 keV was used in order to penetrate the steel capillaries. Room temperature Imaging Plate powder diffraction data were collected on a sample of zeolite Li-A(BW) contained in a steel capillary in an aqueous solution at 200 atm. pressure. With the use of a 10 min exposure, it was possible successfully to refine the crystal structure of zeolite Li-A(BW) using Rietveld refinement. Angle dispersive time-resolved in-situ powder diffraction patterns were collected using a Translating Imaging Plate (TIP) camera. Crystallization and degradation curves for the high-temperature hydrothermal conversion experiments were determined using integrated intensities of selected diffraction lines. The kinetic curves were analyzed using first-order rate expressions.

Authors:
; ; ; ; ;
Publication Date:
Research Org.:
Univ. of Oslo (NO)
Sponsoring Org.:
USDOE; Danish Natural Science Research Council
OSTI Identifier:
20080272
Resource Type:
Journal Article
Journal Name:
Chemistry of Materials
Additional Journal Information:
Journal Volume: 12; Journal Issue: 5; Other Information: PBD: May 2000; Journal ID: ISSN 0897-4756
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; HYDROTHERMAL SYNTHESIS; ALUMINIUM OXIDES; LITHIUM OXIDES; ZEOLITES

Citation Formats

Norby, P., Hanson, J.C., Fitch, A.N., Vaughan, G., Flaks, L., and Gualtieri, A. Formation of {alpha}-eucryptite, LiAlSiO{sub 4}: An in-situ synchrotron X-ray powder diffraction study of a high temperature hydrothermal synthesis. United States: N. p., 2000. Web. doi:10.1021/cm991210h.
Norby, P., Hanson, J.C., Fitch, A.N., Vaughan, G., Flaks, L., & Gualtieri, A. Formation of {alpha}-eucryptite, LiAlSiO{sub 4}: An in-situ synchrotron X-ray powder diffraction study of a high temperature hydrothermal synthesis. United States. doi:10.1021/cm991210h.
Norby, P., Hanson, J.C., Fitch, A.N., Vaughan, G., Flaks, L., and Gualtieri, A. Mon . "Formation of {alpha}-eucryptite, LiAlSiO{sub 4}: An in-situ synchrotron X-ray powder diffraction study of a high temperature hydrothermal synthesis". United States. doi:10.1021/cm991210h.
@article{osti_20080272,
title = {Formation of {alpha}-eucryptite, LiAlSiO{sub 4}: An in-situ synchrotron X-ray powder diffraction study of a high temperature hydrothermal synthesis},
author = {Norby, P. and Hanson, J.C. and Fitch, A.N. and Vaughan, G. and Flaks, L. and Gualtieri, A.},
abstractNote = {Hydrothermal conversion of zeolite Li-A(BW), LiAlSiO{sub 4}{center_dot}H{sub 2}O, into {alpha}-eucryptite, LiAlSiO{sub 4}, occurs at temperatures above 350 C. The authors report here the first in-situ study of a high-temperature hydrothermal synthesis using time-resolved power diffraction. The hydrothermal syntheses were performed in stainless steel capillaries. To maintain hydrothermal conditions, a hydraulic pressure of 2--300 atm was applied. Synchrotron X-ray radiation with energies of 35--40 keV was used in order to penetrate the steel capillaries. Room temperature Imaging Plate powder diffraction data were collected on a sample of zeolite Li-A(BW) contained in a steel capillary in an aqueous solution at 200 atm. pressure. With the use of a 10 min exposure, it was possible successfully to refine the crystal structure of zeolite Li-A(BW) using Rietveld refinement. Angle dispersive time-resolved in-situ powder diffraction patterns were collected using a Translating Imaging Plate (TIP) camera. Crystallization and degradation curves for the high-temperature hydrothermal conversion experiments were determined using integrated intensities of selected diffraction lines. The kinetic curves were analyzed using first-order rate expressions.},
doi = {10.1021/cm991210h},
journal = {Chemistry of Materials},
issn = {0897-4756},
number = 5,
volume = 12,
place = {United States},
year = {2000},
month = {5}
}