Development of a spectro-electrochemical cell for soft X-ray photon-in photon-out spectroscopy

• Published in: Review of scientific instruments Vol. 88; no. 10; p. 104101
• Main Authors: Ishihara, Tomoko, Tokushima, Takashi, Horikawa, Yuka, Kato, Masaru, Yagi, Ichizo
• Format: Journal Article
• Language: English
• Published: United States 01.10.2017
• ISSN: 1089-7623
• DOI: 10.1063/1.4997820

We developed a spectro-electrochemical cell for X-ray absorption and X-ray emission spectroscopy, which are element-specific methods to study local electronic structures in the soft X-ray region. In the usual electrochemical measurement setup, the electrode is placed in solution, and the surface/interface region of the electrode is not normally accessible by soft X-rays that have low penetration depth in liquids. To realize soft X-ray observation of electrochemical reactions, a 15-nm-thick Pt layer was deposited on a 150-nm-thick film window with an adhesive 3-nm-thick Ti layer for use as both the working electrode and the separator window between vacuum and a sample liquid under atmospheric pressure. The designed three-electrode electrochemical cell consists of a Pt film on a SiC window, a platinized Pt wire, and a commercial Ag|AgCl electrode as the working, counter, and reference electrodes, respectively. The functionality of the cell was tested by cyclic voltammetry and X-ray absorption and emission spectroscopy. As a demonstration, the electroplating of Pb on the Pt/SiC membrane window was measured by X-ray absorption and real-time monitoring of fluorescence intensity at the O 1s excitation.