Design and Fabrication of an Electrochemical Cell for X-ray Synchrotron Studies

Presenter: Mazin Hussein

Faculty Sponsor: Sarah L. Perry

School: UMass Amherst

Research Area: Chemical and Biomolecular Engineering

Session: Poster Session 5, 3:15 PM - 4:00 PM, 165, D2

ABSTRACT

Operando electrochemical X-ray absorption spectroscopy (XAS) is used to study electrochemical systems while a voltage is applied, allowing structural and electronic changes to be observed in real time. The reliability of operando measurements depends strongly on the design of the electrochemical cell, which must balance coupled constraints such as X-ray transparency, electrochemical control, and mechanical sealing. Although many operando cell designs are described in the literature, the practical fabrication challenges involved in building and sealing these devices are not discussed in detail. 

This project evaluates whether established operando XAS cell design concepts can be implemented using additive manufacturing and student-accessible fabrication resources at UMass Amherst. A modular three-component sandwich flow cell was designed for fluorescence-mode XAS with a 2.0 mm electrolyte path length and an active volume of approximately 200 µL. The architecture incorporates a Kapton X-ray window, spring-loaded pogo-pin electrical contacts, and a compression-sealed silver pseudo-reference electrode. Structural components were fabricated using fused deposition modeling, and the design was iteratively refined to improve sealing and assembly prior to transitioning to higher-resolution microfluidic printing.

Electrode substrates were fabricated on Kapton using sputtering to produce platinum traces with a defined active area. In parallel, a separate submersible electrode-testing fixture was developed to decouple electrode geometry and contact strategy from the full cell architecture, enabling systematic comparison of working and counter electrode layouts, substrate options, and reference configurations prior to integration into the operando cell.

Overall, this work establishes a structured validation pathway for operando electrochemical cells prior to synchrotron deployment and provides a foundation for future grazing-incidence operando flow-cell designs.

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