Type-II Clathrate Na24-δGe136 from a Redox-Preparation Route
Publikation: Beitrag in Fachzeitschrift › Forschungsartikel › Beigetragen › Begutachtung
Beitragende
Abstract
The metastable type-II clathrate Na24-δGe136 was obtained from Na12Ge17 by applying a two-step procedure. At first, Na12Ge17 was reacted at 70 °C with a solution of benzophenone in the ionic liquid (IL) 1,3-dibutyl-2-methylimidazolium-bis(trifluoromethylsulfonyl) azanide. The IL was inert towards Na12Ge17, but capable of dissolving the sodium salts formed in the redox reaction. By annealing at 340 °C under an argon atmosphere, the X-ray amorphous intermediate product was transformed to crystalline Na24-δGe136 (δ≈2) and α-Ge in an about 1 : 1 mass ratio. The product was characterized by X-ray powder diffraction, chemical analysis, and 23Na solid-state NMR spectroscopy. Metallic properties of Na24-δGe136 were revealed by a significant Knight shift of the 23Na NMR signals and by a Pauli-paramagnetic contribution to the magnetic susceptibility. At room temperature, Na24-δGe136 slowly ages, with a tendency to volume decrease and sodium loss.
Details
Originalsprache | Englisch |
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Seiten (von - bis) | 12776-12787 |
Seitenumfang | 12 |
Fachzeitschrift | Chemistry - A European Journal |
Jahrgang | 27 |
Ausgabenummer | 50 |
Publikationsstatus | Veröffentlicht - 6 Sept. 2021 |
Peer-Review-Status | Ja |
Externe IDs
PubMed | 34270132 |
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Schlagworte
ASJC Scopus Sachgebiete
Schlagwörter
- intermetallic clathrates, ionic liquids, metastable compounds, redox chemistry, Zintl phases