Locating Gases in Porous Materials: Cryogenic Loading of Fuel-Related Gases Into a Sc-based Metal-Organic Framework under Extreme Pressures

An alternative approach to loading metal organic frameworks with gas molecules at high (kbar) pressures is reported. The technique, which uses liquefied gases as pressure transmitting media within a diamond anvil cell along with a single‐crystal of a porous metal–organic framework, is demonstrated t...

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Bibliographic Details
Published in:Angewandte Chemie 2015-11, Vol.127 (45), p.13530-13534
Main Authors: Sotelo, Jorge, Woodall, Christopher H., Allan, Dave R., Gregoryanz, Eugene, Howie, Ross T., Kamenev, Konstantin V., Probert, Michael R., Wright, Paul A., Moggach, Stephen A.
Format: Article
Language:English
Subjects:
Adsorption
Carbon dioxide
Chemistry
Diamond anvil cells
Gases
Gastrennung
Hochdruckphasen
Isotherms
Liquefied
Liquefied gases
Metal-organic frameworks
Metall-organische Gerüstverbindungen
Metalorganic compounds
Metals
Phase transitions
Porous materials
Pressure
Röntgenkristallographie
Strukturaufklärung
Transmission
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Summary:An alternative approach to loading metal organic frameworks with gas molecules at high (kbar) pressures is reported. The technique, which uses liquefied gases as pressure transmitting media within a diamond anvil cell along with a single‐crystal of a porous metal–organic framework, is demonstrated to have considerable advantages over other gas‐loading methods when investigating host–guest interactions. Specifically, loading the metal–organic framework Sc2BDC3 with liquefied CO2 at 2 kbar reveals the presence of three adsorption sites, one previously unreported, and resolves previous inconsistencies between structural data and adsorption isotherms. A further study with supercritical CH4 at 3–25 kbar demonstrates hyperfilling of the Sc2BDC3 and two high‐pressure displacive and reversible phase transitions are induced as the filled MOF adapts to reduce the volume of the system. Die maximale Gasaufnahme von porösen Metall‐organischen Gerüsten (MOFs) kann durch die Verwendung von Gasen als druckübertragenden Medien in Hochdruck‐Röntgenbeugungsexperimenten untersucht werden. Eine Studie mit überkritischem CH4 bei 3–25 kbar demonstriert das Auftreten zweier Hochdruckphasenübergänge, da das MOF durch Volumenreduktion auf die Gasadsorption reagiert.
ISSN:0044-8249
1521-3757
DOI:10.1002/ange.201506250