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Fabrication and testing of an electrochemical microcell for in situ soft X-ray microspectroscopy measurements

DOI: 10.1088/1742-6596/425/18/182010 DOI Help

Authors: A. Gianoncelli (Elettra - Sinctrotrone Trieste) , B. Kaulich (Diamond Light Source) , M. Kiskinova (Elettra - Sinctrotrone Trieste) , C. Mele (Università di Lecce) , M. Prasciolu (DESY) , I. Sgura (Università di Lecce) , B. Bozzini (Università di Lecce)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Journal Of Physics: Conference Series , VOL 425 (18)

State: Published (Approved)
Published: March 2013

Abstract: In this paper we report on the fabrication and testing of a novel concept of electrochemical microcell for in-situ soft X-ray microspectroscopy in transmission. The microcell, fabricated by electron-beam lithography, implements an improved electrode design, with optimal current density distribution and minimised ohmic drop, allowing the same three-electrode electrochemical control achievable with traditional cells. Moreover standard electroanalytical measurements, such as cyclic voltammetry, can be routinely performed. As far as the electrolyte is concerned, we selected a room-temperature ionic-liquid. Some of the materials belonging to this class, in addition to a broad range of outstanding electrochemical properties, feature two highlights that are crucial for in situ, soft X-ray transmission work: spinnability, enabling accurate thickness control, and stability to UHV, allowing operation of an open cell in the analysis chamber vacuum (10−6 mbar). The cell can, of course, be used also with non-vacuum stable electrolytes in the sealed version developed in previous work in our group. In this study, the microcell designed, fabricated and tested in situ by applying an anodic polarisation to a Au electrode and following the formation of a distribution of corrosion features. This specific material combination presented in this work does not limit the cell concept, that can implement any electrodic material grown by lithography, any liquid electrolyte and any spinnable solid electrolyte.

Journal Keywords: Corrosion; Current Density; Design; Distribution; Electrochemistry; Electrodes; Electron Beams; Fabrication; Polarization; Soft X Radiation; Solid Electrolytes; Stability; Standards; Temperature Range 0273-0400 K; Testing; Transmission; Voltametry

Subject Areas: Physics


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