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Published October 14, 2019 | Supplemental Material
Journal Article Open

Scanning electrochemical flow cell with online mass spectroscopy for accelerated screening of carbon dioxide reduction electrocatalysts

Abstract

Electrochemical conversion of carbon dioxide into valuable chemicals or fuels is an increasingly important strategy for achieving carbon neutral technologies. The lack of a sufficiently active and selective electrocatalyst, particularly for synthesizing highly reduced products, motivates accelerated screening to evaluate new catalyst spaces. Traditional techniques, which couple electrocatalyst operation with analytical techniques to measure product distributions, enable screening throughput at 1–10 catalysts per day. In this paper, a combinatorial screening instrument is designed for MS detection of hydrogen, methane, and ethylene in quasi-real-time during catalyst operation experiments in an electrochemical flow cell. Coupled with experiment modeling, product detection during cyclic voltammetry (CV) enables modeling of the voltage-dependent partial current density for each detected product. We demonstrate the technique by using the well-established thin film Cu catalysts and by screening a Pd–Zn composition library in carbonate-buffered aqueous electrolyte. The rapid product distribution characterization over a large range of overpotential makes the instrument uniquely suited for accelerating screening of electrocatalysts for the carbon dioxide reduction reaction.

Additional Information

© 2019 American Chemical Society. Received: July 12, 2019; Revised: September 11, 2019; Published: September 16, 2019. This material is based upon work performed by the Joint Center for Artificial Photosynthesis, a DOE Energy Innovation Hub, supported through the Office of Science of the U.S. Department of Energy (Award No. DE-SC0004993). Use of the Stanford Synchrotron Radiation Lightsource, SLAC National Accelerator Laboratory, is supported by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences, under Contract No. DE-AC02-76SF00515. The authors thank Apurva Mehta and Douglas G. Van Campen for assistance with collection of synchrotron XRD data. The authors declare no competing financial interest.

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