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

作者：Salas Colera Eduardo; Munoz Noval Alvaro; Heyman Catherine; Ania Conchi O; Parra Jose B; Garcia Granda Santiago; Calero Sofia; Rubio Zuazo Juan; Castro German R^*

来源：JOURNAL OF SYNCHROTRON RADIATION, 2015, 22(1): 42-48.

DOI：10.1107/S1600577514021018

• X-ray powder diffraction
• isobaric/isothermal environment

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.

• 出版日期2015-1