In this paper we introduce a microelectrochemical cell configured for generation-collection experiments and designed primarily for examining the kinetics of electrocatalysts. The heart of the device consists of two, closely spaced, pyrolyzed photoresist microband electrodes enclosed within a microchannel. The cell is suitable for evaluating the efficiency of electrocatalysts under an unprecedented range of conditions. Specifically, compared to the gold-standard rotating ring-disk electrode (RRDE), this device offers four major advantages. First, collection efficiencies of 97% are easily achieved, compared to values of 20–37% that are characteristic of RRDEs. Second, mass transfer coefficients of 0.5 cm s−1 are accessible for typical redox species, which is significantly higher than RRDEs (up to 0.01 cm s−1). Third, we show that the device can operate effectively at temperatures up to 70 °C, which is important for measuring electrochemical kinetics that are relevant to fuel cell catalysts. Finally, much less catalyst and much smaller volumes of electrolyte solution are required to make kinetic measurements using the microelectrochemical device compared to the RRDE. Here, we present the simple procedure used to fabricate the device, fundamental electroanalytical characterization, and electrocatalytic measurements relevant to the oxygen reduction reaction.
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