Open AccessDesign 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
Author(s) -
SalasColera Eduardo,
MuñozNoval Álvaro,
Heyman Catherine,
Ania Conchi O.,
Parra José B.,
GarcíaGranda Santiago,
Calero Sofía,
RubioZuazo Juan,
Castro Germán R.
Publication year - 2015
Publication title -
journal of synchrotron radiation
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.172
H-Index - 99
ISSN - 1600-5775
DOI - 10.1107/s1600577514021018
Subject(s) - isobaric process , isothermal process , powder diffraction , synchrotron , diffraction , adsorption , materials science , synchrotron radiation , x ray crystallography , analytical chemistry (journal) , chemistry , thermodynamics , crystallography , optics , chromatography , physics
A 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 N 2 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.