title: 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.
abstract: 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 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.
authors.affiliation: SpLine, Spanish CRG BM25 Beamline, ESRF, 6 rue Jules Horowitz, 38000 Grenoble, France.
authors.forename: Eduardo
authors.initials: E
authors.lastname: Salas-Colera
authors.affiliation: SpLine, Spanish CRG BM25 Beamline, ESRF, 6 rue Jules Horowitz, 38000 Grenoble, France.
authors.forename: Álvaro
authors.initials: Á
authors.lastname: Muñoz-Noval
authors.affiliation: CAO-DAO Heyman, 5 place de Gordes, 38000 Grenoble, France.
authors.forename: Catherine
authors.initials: C
authors.lastname: Heyman
authors.affiliation: ADPOR Group, Instituto Nacional del Carbón (INCAR, CSIC), Oviedo, Spain.
authors.forename: Conchi O
authors.initials: CO
authors.lastname: Ania
authors.affiliation: ADPOR Group, Instituto Nacional del Carbón (INCAR, CSIC), Oviedo, Spain.
authors.forename: José B
authors.initials: JB
authors.lastname: Parra
authors.affiliation: CAO-DAO Heyman, 5 place de Gordes, 38000 Grenoble, France.
authors.forename: Santiago
authors.initials: S
authors.lastname: García-Granda
authors.affiliation: Department of Physical, Chemical and Natural Systems, University Pablo de Olavide, Seville, Spain.
authors.forename: Sofía
authors.initials: S
authors.lastname: Calero
authors.affiliation: SpLine, Spanish CRG BM25 Beamline, ESRF, 6 rue Jules Horowitz, 38000 Grenoble, France.
authors.forename: Juan
authors.initials: J
authors.lastname: Rubio-Zuazo
authors.affiliation: SpLine, Spanish CRG BM25 Beamline, ESRF, 6 rue Jules Horowitz, 38000 Grenoble, France.
authors.forename: Germán R
authors.initials: GR
authors.lastname: Castro
keywords: X-ray powder diffraction; isobaric/isothermal environment