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Koop, T., Schindler, W., Kazimirov, A., Scherb, G., Zegenhagen, J., Schulz, Th., Feidenhans'l, R., Kirschner, J.

Electrochemical cell for in situ X-ray diffraction under ultrapure conditions
Review of Scientific Instruments 69, (4),pp 1840-1843 (1998)
An electrochemical cell has been developed for in situ x-ray diffraction from a working electrode under clean conditions equivalent to ultrahigh vacuum conditions of 5 x 10−10 mbar. The substrate crystals can be prepared ex situ and transferred into the cell under protection of ultrapure water within a few seconds. The oxygen level in the electrolyte is reduced by continuous N2 flow to less than 0.2% compared to that of a fresh electrolyte. This can be done while rotating the cell by 360° about the surface normal. The electrode potential is accurately measured at the position of the crystal using a Luggin capillary and a standard reference electrode. We demonstrate the performance of our cell by in situ synchrotron x-ray diffraction measurements on ultrathin Co layers electrodeposited on Cu(001) in an aqueous H2SO4/CoSO4 solution.

ki-1998-e01