Spectroscopic studies are rarely performed at very high temperature, especially when combined with light from a synchrotron source. Demanding conditions of maintaining ultrahigh vacuum (UHV) during heating, together with the typically brief access to beam time at multiuser synchrotron end stations, may contribute to some of the reasons for the difficulty of such experiments. Consequently, a large number of materials with interesting properties and industrial applications at high temperature remain unexplored. The authors describe here a simple portable sample mount assembly that can be easily utilized at a beamline, with potential utility for a variety of spectroscopic measurements requiring elevated temperatures and an UHV environment. In the specific application described here, the authors use a resistive cartridge heater interfaced with a standard manipulator previously designed for cooling by liquid nitrogen with an UHV chamber and a cylindrical mirror analyzer for x-ray photoemission spectroscopy (XPS) [also known as electron spectroscopy for chemical analysis (ESCA)] at the Synchrotron Radiation Center in Stoughton, WI. The heater cartridge required only modest power to reach target temperatures using an open-loop temperature control. Finally, the authors describe the measurements of XPS (ESCA) and total-electron yield x-ray absorption spectroscopy on nanopowders and on single crystals grown by them. They emphasize the simplicity of the setup, which they believe would be of interest to groups performing measurements at large facilities, where access and time are both limited.
Ultrahigh vacuum sample mount for x-ray photoelectron spectroscopy up to very high temperature (150–1400 K)
Mark S. Williamsen, Shishir K. Ray, Ying Zou, John A. Dudek, Somaditya Sen, Mark Bissen, Laura Kretsch, Vaijayanti R. Palkar, Marshall F. Onellion, Prasenjit Guptasarma; Ultrahigh vacuum sample mount for x-ray photoelectron spectroscopy up to very high temperature (150–1400 K). J. Vac. Sci. Technol. A 1 May 2011; 29 (3): 031602. https://doi.org/10.1116/1.3571528
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