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Design and development of a controlled pressure/temperature set-up for in situ studies of solid–gas processes and reactions in a synchrotron X-ray powder diffraction station

AutorSalas-Colera, E.; Muñoz-Noval, Á.; Heyman, C.; Ovín Ania, María Concepción ; Parra Soto, José Bernardo ; García-Granda, Santiago ; Calero, S.; Rubio-Zuazo, J. ; Castro, Germán R.
Palabras claveX-ray powder diffraction
Isobaric/isothermal environment
Fecha de publicaciónene-2015
EditorWiley-VCH
CitaciónJournal of Synchrotron Radiation 22(1): 42-48 (2015)
ResumenA novel set-up has been designed and used for synchrotron radiation X-ray high-resolution powder diffraction (SR-HRPD) in transmission geometry (spinning capillary) for in situ solid–gas reactions and processes in an isobaric and isothermal environment. The pressure and temperature of the sample are controlled from 10−3 to 1000 mbar and from 80 to 1000 K, respectively. To test the capacities of this novel experimental set-up, structure deformation in the porous material zeolitic imidazole framework (ZIF-8) by gas adsorption at cryogenic temperature has been studied under isothermal and isobaric conditions. Direct structure deformations by the adsorption of Ar and N2 gases have been observed in situ, demonstrating that this set-up is perfectly suitable for direct structural analysis under in operando conditions. The presented results prove the feasibility of this novel experimental station for the characterization in real time of solid–gas reactions and other solid–gas processes by SR-HRPD.
Versión del editorhttp://dx.doi.org/10.1107/S1600577514021018
URIhttp://hdl.handle.net/10261/123294
DOI10.1107/S1600577514021018
ISSN0909-0495
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