Details
| Original language | English |
|---|---|
| Pages (from-to) | 54-61 |
| Number of pages | 8 |
| Journal | Microporous and Mesoporous Materials |
| Volume | 174 |
| Early online date | 7 Mar 2013 |
| Publication status | Published - 1 Jul 2013 |
Abstract
Tetrahydroborate enclathrated gallogermanate sodalite was successfully synthesized under mild hydrothermal conditions and characterized by X-ray powder diffraction and Fourier transform infrared (FTIR) spectroscopy. The crystal structure was refined in space group P4̄3n using the Rietveld method: a = 912.581(1) pm, V = 760.0(1) · 10-6 pm3, R B = 0.019. Within the sodalite cage formed by corner-sharing oxygen coordinated gallium and germanium tetrahedra, the hydrogen atoms of the enclathrated BH4 - anions were refined on 8e (x, x, x) crystallographic position. The boron-hydrogen distances were restrained to 124.7 pm as calculated from the respective bond valence sums. High temperature behavior was investigated using temperature-dependent X-ray diffraction, FTIR and Raman spectroscopy and TG-DTA methods. A two-step sodalite decomposition reaction to the beryllonite analogous phase NaGaGeO4 was observed. The temperature-dependent development of the sodalite structural parameters evaluated by Rietveld analysis of the XRD data indicate a beginning transformation of the enclathrated NaBH4 at about 528 K followed by a decomposition of the sodalite framework starting at about 648 K. These findings are confirmed by the results obtained from temperature-dependent Raman and FTIR data evaluation.
Keywords
- Crystal structure, Gallogermanates, Sodalite, Synthesis, Thermal behavior
ASJC Scopus subject areas
- Chemistry(all)
- General Chemistry
- Materials Science(all)
- General Materials Science
- Physics and Astronomy(all)
- Condensed Matter Physics
- Engineering(all)
- Mechanics of Materials
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In: Microporous and Mesoporous Materials, Vol. 174, 01.07.2013, p. 54-61.
Research output: Contribution to journal › Article › Research › peer review
}
TY - JOUR
T1 - Synthesis, crystal structure and temperature-dependent behavior of gallogermanate tetrahydroborate sodalite |Na8(BH4) 2|[GaGeO4]6
AU - Poltz, Irma
AU - Robben, Lars
AU - Buhl, Josef Christian
AU - Gesing, Thorsten M.
N1 - Funding Information: We gratefully acknowledge the Deutsche Forschungsgemeinschaft (DFG) for the financial support of Heisenberg project GE1981/3-1. Additionally, we like to thank Dr. I. Reese and Dr. B. Bleisteiner (HORIBA Europe GmbH, Darmstadt, Germany) for carrying out the TD-Raman measurements.
PY - 2013/7/1
Y1 - 2013/7/1
N2 - Tetrahydroborate enclathrated gallogermanate sodalite was successfully synthesized under mild hydrothermal conditions and characterized by X-ray powder diffraction and Fourier transform infrared (FTIR) spectroscopy. The crystal structure was refined in space group P4̄3n using the Rietveld method: a = 912.581(1) pm, V = 760.0(1) · 10-6 pm3, R B = 0.019. Within the sodalite cage formed by corner-sharing oxygen coordinated gallium and germanium tetrahedra, the hydrogen atoms of the enclathrated BH4 - anions were refined on 8e (x, x, x) crystallographic position. The boron-hydrogen distances were restrained to 124.7 pm as calculated from the respective bond valence sums. High temperature behavior was investigated using temperature-dependent X-ray diffraction, FTIR and Raman spectroscopy and TG-DTA methods. A two-step sodalite decomposition reaction to the beryllonite analogous phase NaGaGeO4 was observed. The temperature-dependent development of the sodalite structural parameters evaluated by Rietveld analysis of the XRD data indicate a beginning transformation of the enclathrated NaBH4 at about 528 K followed by a decomposition of the sodalite framework starting at about 648 K. These findings are confirmed by the results obtained from temperature-dependent Raman and FTIR data evaluation.
AB - Tetrahydroborate enclathrated gallogermanate sodalite was successfully synthesized under mild hydrothermal conditions and characterized by X-ray powder diffraction and Fourier transform infrared (FTIR) spectroscopy. The crystal structure was refined in space group P4̄3n using the Rietveld method: a = 912.581(1) pm, V = 760.0(1) · 10-6 pm3, R B = 0.019. Within the sodalite cage formed by corner-sharing oxygen coordinated gallium and germanium tetrahedra, the hydrogen atoms of the enclathrated BH4 - anions were refined on 8e (x, x, x) crystallographic position. The boron-hydrogen distances were restrained to 124.7 pm as calculated from the respective bond valence sums. High temperature behavior was investigated using temperature-dependent X-ray diffraction, FTIR and Raman spectroscopy and TG-DTA methods. A two-step sodalite decomposition reaction to the beryllonite analogous phase NaGaGeO4 was observed. The temperature-dependent development of the sodalite structural parameters evaluated by Rietveld analysis of the XRD data indicate a beginning transformation of the enclathrated NaBH4 at about 528 K followed by a decomposition of the sodalite framework starting at about 648 K. These findings are confirmed by the results obtained from temperature-dependent Raman and FTIR data evaluation.
KW - Crystal structure
KW - Gallogermanates
KW - Sodalite
KW - Synthesis
KW - Thermal behavior
UR - http://www.scopus.com/inward/record.url?scp=84875706975&partnerID=8YFLogxK
U2 - 10.1016/j.micromeso.2013.02.038
DO - 10.1016/j.micromeso.2013.02.038
M3 - Article
AN - SCOPUS:84875706975
VL - 174
SP - 54
EP - 61
JO - Microporous and Mesoporous Materials
JF - Microporous and Mesoporous Materials
SN - 1387-1811
ER -