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Title: Formation pathway, structural characterization and optimum processing parameters of synthetic topaz – Al{sub 2}SiO{sub 4}(OH,F){sub 2} – by CVD

Abstract

A novel synthesis route for topaz (Al{sub 2}SiO{sub 4}(OH,F){sub 2}) by chemical vapor deposition (CVD) using Na{sub 2}SiF{sub 6} as solid precursor was developed. Synthesis tests were conducted with and without a flow of nitrogen, positioning the Al(OH){sub 3} substrate at 0° and 90° with respect to the gas flow direction, at 700 and 750 °C, for 60 and 90 min, respectively. It was found that topaz is synthesized through two pathways, directly and indirectly, involving a series of endothermic and exothermic, heterogeneous and homogeneous reactions between Al(OH){sub 3} and SiF{sub 4}(g). Analytical structural determination confirmed existence of orthorhombic polycrystals with lattice parameters of a =4.6558 Å, b=8.8451 Å and c=8.4069 Å. According to ANOVA, while temperature, time and interaction of substrate angular position with atmosphere (P×A) are the parameters that most significantly influence the variability in the amount of topaz formed – equivalent contributions of 31% – topaz lattice parameters are mostly impacted by the same factors (T, t, P, A), but without the interaction factor. The projected amount of topaz is in good agreement with that obtained in confirmation tests under optimal conditions: Al(OH){sub 3} substrate compact placed at 0°, treated at 750 °C for 90 min inmore » the absence of N{sub 2}. - Highlights: • Topaz synthesis as a unique phase by CVD, using solid precursor Na{sub 2}SiF{sub 6} is feasible. • Two pathways, a series of endothermic/exothermic, heterogeneous/homogeneous reactions. • Crystal structure, orthorhombic polycrystals: a =4.6558 Å, b=8.8451 Å, c=8.4069 Å. • Anova: amount of topaz formed and lattice parameters are impacted by same factors. • Projection of topaz quantity in good agreement with those from confirmation tests.« less

Authors:
;
Publication Date:
OSTI Identifier:
22486823
Resource Type:
Journal Article
Journal Name:
Journal of Solid State Chemistry
Additional Journal Information:
Journal Volume: 230; Other Information: Copyright (c) 2015 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; Country of input: International Atomic Energy Agency (IAEA); Journal ID: ISSN 0022-4596
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; ALUMINIUM HYDROXIDES; ALUMINIUM SILICATES; CHEMICAL VAPOR DEPOSITION; GAS FLOW; LATTICE PARAMETERS; NITROGEN; ORTHORHOMBIC LATTICES; POLYCRYSTALS; PRECURSOR; SILICON FLUORIDES; SOLIDS; SUBSTRATES; SYNTHESIS

Citation Formats

Trujillo-Vázquez, E., E-mail: evatrujillo87@gmail.com, and Pech-Canul, M.I., E-mail: martin.pech@cinvestav.edu.mx. Formation pathway, structural characterization and optimum processing parameters of synthetic topaz – Al{sub 2}SiO{sub 4}(OH,F){sub 2} – by CVD. United States: N. p., 2015. Web. doi:10.1016/J.JSSC.2015.07.030.
Trujillo-Vázquez, E., E-mail: evatrujillo87@gmail.com, & Pech-Canul, M.I., E-mail: martin.pech@cinvestav.edu.mx. Formation pathway, structural characterization and optimum processing parameters of synthetic topaz – Al{sub 2}SiO{sub 4}(OH,F){sub 2} – by CVD. United States. https://doi.org/10.1016/J.JSSC.2015.07.030
Trujillo-Vázquez, E., E-mail: evatrujillo87@gmail.com, and Pech-Canul, M.I., E-mail: martin.pech@cinvestav.edu.mx. 2015. "Formation pathway, structural characterization and optimum processing parameters of synthetic topaz – Al{sub 2}SiO{sub 4}(OH,F){sub 2} – by CVD". United States. https://doi.org/10.1016/J.JSSC.2015.07.030.
@article{osti_22486823,
title = {Formation pathway, structural characterization and optimum processing parameters of synthetic topaz – Al{sub 2}SiO{sub 4}(OH,F){sub 2} – by CVD},
author = {Trujillo-Vázquez, E., E-mail: evatrujillo87@gmail.com and Pech-Canul, M.I., E-mail: martin.pech@cinvestav.edu.mx},
abstractNote = {A novel synthesis route for topaz (Al{sub 2}SiO{sub 4}(OH,F){sub 2}) by chemical vapor deposition (CVD) using Na{sub 2}SiF{sub 6} as solid precursor was developed. Synthesis tests were conducted with and without a flow of nitrogen, positioning the Al(OH){sub 3} substrate at 0° and 90° with respect to the gas flow direction, at 700 and 750 °C, for 60 and 90 min, respectively. It was found that topaz is synthesized through two pathways, directly and indirectly, involving a series of endothermic and exothermic, heterogeneous and homogeneous reactions between Al(OH){sub 3} and SiF{sub 4}(g). Analytical structural determination confirmed existence of orthorhombic polycrystals with lattice parameters of a =4.6558 Å, b=8.8451 Å and c=8.4069 Å. According to ANOVA, while temperature, time and interaction of substrate angular position with atmosphere (P×A) are the parameters that most significantly influence the variability in the amount of topaz formed – equivalent contributions of 31% – topaz lattice parameters are mostly impacted by the same factors (T, t, P, A), but without the interaction factor. The projected amount of topaz is in good agreement with that obtained in confirmation tests under optimal conditions: Al(OH){sub 3} substrate compact placed at 0°, treated at 750 °C for 90 min in the absence of N{sub 2}. - Highlights: • Topaz synthesis as a unique phase by CVD, using solid precursor Na{sub 2}SiF{sub 6} is feasible. • Two pathways, a series of endothermic/exothermic, heterogeneous/homogeneous reactions. • Crystal structure, orthorhombic polycrystals: a =4.6558 Å, b=8.8451 Å, c=8.4069 Å. • Anova: amount of topaz formed and lattice parameters are impacted by same factors. • Projection of topaz quantity in good agreement with those from confirmation tests.},
doi = {10.1016/J.JSSC.2015.07.030},
url = {https://www.osti.gov/biblio/22486823}, journal = {Journal of Solid State Chemistry},
issn = {0022-4596},
number = ,
volume = 230,
place = {United States},
year = {Thu Oct 15 00:00:00 EDT 2015},
month = {Thu Oct 15 00:00:00 EDT 2015}
}