A capillary sample cell used for in-situ SAXS, XRD, and XAFS measurements during hydrothermal synthesis.

Hydrothermal synthesis was extensively used for the material preparation. In this paper, a capillary sample cell was designed for in-situ small angle X-ray scattering (SAXS), X-ray diffraction (XRD), and X-ray absorption fine structure (XAFS) studies during hydrothermal synthesis. Kalrez sealing ring was used to seal the liquid sample into a capillary. CO 2 or inert gases were used as the pressure transmitting medium. A three-way valve was used to switch the liquid sample or the pressure transmitting medium. Sheathed heat-blocks were used to heat the capillary. The hydrothermal pressure can be up to 4.0 ± 0.1 MPa, and the hydrothermal temperature can reach to 600 ± 1 K. In-situ SAXS, XRD, and XAFS measurements during the hydrothermal synthesis of bismuth carbonate oxide confirm the feasibility that the capillary sample cell can be used for real-time structural characterization. Its application in Beijing Synchrotron Radiation Facility is expected to provide users with a new experimental research means. [ABSTRACT FROM AUTHOR]