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Title: MAS-NMR studies of lithium aluminum silicate (LAS) glasses and glass-ceramics having different Li{sub 2}O/Al{sub 2}O{sub 3} ratio

Abstract

Emergence of phases in lithium aluminum silicate (LAS) glasses of composition (wt%) xLi{sub 2}O-71.7SiO{sub 2}-(17.7-x)Al{sub 2}O{sub 3}-4.9K{sub 2}O-3.2B{sub 2}O{sub 3}-2.5P{sub 2}O{sub 5} (5.1<=x<=12.6) upon heat treatment were studied. {sup 29}Si, {sup 27}Al, {sup 31}P and {sup 11}B MAS-NMR were employed for structural characterization of both LAS glasses and glass-ceramics. In glass samples, Al is found in tetrahedral coordination, while P exists mainly in the form of orthophosphate units. B exists as BO{sub 3} and BO{sub 4} units. {sup 27}Al NMR spectra show no change with crystallization, ruling out the presence of any Al containing phase. Contrary to X-ray diffraction studies carried out, {sup 11}B (high field 18.8 T) and {sup 29}Si NMR spectra clearly indicate the unexpected crystallization of a borosilicate phase (Li,K)BSi{sub 2}O{sub 6}, whose structure is similar to the aluminosilicate virgilite. Also, lithium disilicate (Li{sub 2}Si{sub 2}O{sub 5}), lithium metasilicate (Li{sub 2}SiO{sub 3}) and quartz (SiO{sub 2}) were identified in the {sup 29}Si NMR spectra of the glass-ceramics. {sup 31}P NMR spectra of the glass-ceramics revealed the presence of Li{sub 3}PO{sub 4} and a mixed phase (Li,K){sub 3}PO{sub 4} at low alkali concentrations. - Graphical Abstract: The {sup 11}B MAS-NMR spectra of lithium aluminum silicate (LAS) glass-ceramics indicatingmore » the formation of Li/KBSiO{sub 6} phase. This phase is isostructural with virgilite and cannot be distinguished in X-ray diffractograms.« less

Authors:
 [1]; ;  [2]
  1. Technical Physics and Prototype Engineering Division, Bhabha Atomic Research Centre, Mumbai 400085 (India)
  2. UCCS - Unite de Catalyse et Chimie du Solide - UMR CNRS 8181, Ecole Nationale Superieure de Chimie de Lille, Universite des Sciences et Technologies de Lille, BP 108, 59562 Villeneuve d'Ascq Cedex (France)
Publication Date:
OSTI Identifier:
21372457
Resource Type:
Journal Article
Journal Name:
Journal of Solid State Chemistry
Additional Journal Information:
Journal Volume: 183; Journal Issue: 1; Other Information: DOI: 10.1016/j.jssc.2009.10.006; PII: S0022-4596(09)00488-5; Copyright (c) 2009 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; Journal ID: ISSN 0022-4596
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; ALUMINIUM OXIDES; ALUMINIUM SILICATES; BORATES; BORON SILICATES; CERAMICS; CRYSTALLIZATION; GLASS; HEAT TREATMENTS; LITHIUM OXIDES; LITHIUM PHOSPHATES; LITHIUM SILICATES; NMR SPECTRA; QUARTZ; SILICON OXIDES; X-RAY DIFFRACTION; ALKALI METAL COMPOUNDS; ALUMINIUM COMPOUNDS; BORON COMPOUNDS; CHALCOGENIDES; COHERENT SCATTERING; DIFFRACTION; LITHIUM COMPOUNDS; MINERALS; OXIDE MINERALS; OXIDES; OXYGEN COMPOUNDS; PHASE TRANSFORMATIONS; PHOSPHATES; PHOSPHORUS COMPOUNDS; SCATTERING; SILICATES; SILICON COMPOUNDS; SPECTRA

Citation Formats

Ananthanarayanan, A, Kothiyal, G.P., E-mail: gpkoth@barc.gov.i, Montagne, L, and Revel, B. MAS-NMR studies of lithium aluminum silicate (LAS) glasses and glass-ceramics having different Li{sub 2}O/Al{sub 2}O{sub 3} ratio. United States: N. p., 2010. Web. doi:10.1016/j.jssc.2009.10.006.
Ananthanarayanan, A, Kothiyal, G.P., E-mail: gpkoth@barc.gov.i, Montagne, L, & Revel, B. MAS-NMR studies of lithium aluminum silicate (LAS) glasses and glass-ceramics having different Li{sub 2}O/Al{sub 2}O{sub 3} ratio. United States. https://doi.org/10.1016/j.jssc.2009.10.006
Ananthanarayanan, A, Kothiyal, G.P., E-mail: gpkoth@barc.gov.i, Montagne, L, and Revel, B. 2010. "MAS-NMR studies of lithium aluminum silicate (LAS) glasses and glass-ceramics having different Li{sub 2}O/Al{sub 2}O{sub 3} ratio". United States. https://doi.org/10.1016/j.jssc.2009.10.006.
@article{osti_21372457,
title = {MAS-NMR studies of lithium aluminum silicate (LAS) glasses and glass-ceramics having different Li{sub 2}O/Al{sub 2}O{sub 3} ratio},
author = {Ananthanarayanan, A and Kothiyal, G.P., E-mail: gpkoth@barc.gov.i and Montagne, L and Revel, B},
abstractNote = {Emergence of phases in lithium aluminum silicate (LAS) glasses of composition (wt%) xLi{sub 2}O-71.7SiO{sub 2}-(17.7-x)Al{sub 2}O{sub 3}-4.9K{sub 2}O-3.2B{sub 2}O{sub 3}-2.5P{sub 2}O{sub 5} (5.1<=x<=12.6) upon heat treatment were studied. {sup 29}Si, {sup 27}Al, {sup 31}P and {sup 11}B MAS-NMR were employed for structural characterization of both LAS glasses and glass-ceramics. In glass samples, Al is found in tetrahedral coordination, while P exists mainly in the form of orthophosphate units. B exists as BO{sub 3} and BO{sub 4} units. {sup 27}Al NMR spectra show no change with crystallization, ruling out the presence of any Al containing phase. Contrary to X-ray diffraction studies carried out, {sup 11}B (high field 18.8 T) and {sup 29}Si NMR spectra clearly indicate the unexpected crystallization of a borosilicate phase (Li,K)BSi{sub 2}O{sub 6}, whose structure is similar to the aluminosilicate virgilite. Also, lithium disilicate (Li{sub 2}Si{sub 2}O{sub 5}), lithium metasilicate (Li{sub 2}SiO{sub 3}) and quartz (SiO{sub 2}) were identified in the {sup 29}Si NMR spectra of the glass-ceramics. {sup 31}P NMR spectra of the glass-ceramics revealed the presence of Li{sub 3}PO{sub 4} and a mixed phase (Li,K){sub 3}PO{sub 4} at low alkali concentrations. - Graphical Abstract: The {sup 11}B MAS-NMR spectra of lithium aluminum silicate (LAS) glass-ceramics indicating the formation of Li/KBSiO{sub 6} phase. This phase is isostructural with virgilite and cannot be distinguished in X-ray diffractograms.},
doi = {10.1016/j.jssc.2009.10.006},
url = {https://www.osti.gov/biblio/21372457}, journal = {Journal of Solid State Chemistry},
issn = {0022-4596},
number = 1,
volume = 183,
place = {United States},
year = {Fri Jan 15 00:00:00 EST 2010},
month = {Fri Jan 15 00:00:00 EST 2010}
}