Controlled sample environment for studying solid-gas interactions by in situ powder X-ray diffraction

Abstract

A sample cell for powder X-ray diffraction studies with in situ applied pressure and control of temperature is demonstrated. The cell is based on a previously reported design and consists of a glass or quartz capillary glued into a Swagelok weld gland; this configuration can hold up to 100 bar (1 bar = 100 kPa). The cell is placed in contact with a copper plate for control of temperature between -30 and 200°C. This is achieved by Peltier elements, heat cartridges and a refrigerated circulating bath. This work mainly focuses on the temperature control system. Commissioning tests were performed in a custom-made small/wide-angle X-ray diffractometer at the Norwegian University of Science and Technology. The system is easily portable to synchrotron facilities.

Keywords: powder diffraction; pressure; sample cell; temperature.