Electrocatalytic Activity of Pd−Co Bimetallic Mixtures for Formic Acid Oxidation Studied by Scanning Electrochemical Microscopy

The electrochemical oxidation of formic acid was studied by the tip generation-substrate collection (TG-SC) mode of scanning electrochemical microscopy (SECM), extending the number of applications of SECM in electrocatalysis. Formic acid was generated at a Hg on Au ultramicroelectrode (UME) tip by r...

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Bibliographic Details
Published in:Analytical chemistry (Washington) 2009-08, Vol.81 (16), p.7003-7008
Main Authors: Jung, Changhoon, Sánchez-Sánchez, Carlos M, Lin, Cheng-Lan, Rodríguez-López, Joaquín, Bard, Allen J
Format: Article
Language:English
Subjects:
Analytical chemistry
Chemistry
Chromatographic methods and physical methods associated with chromatography
Electrochemical methods
Exact sciences and technology
Gas chromatographic methods
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Summary:The electrochemical oxidation of formic acid was studied by the tip generation-substrate collection (TG-SC) mode of scanning electrochemical microscopy (SECM), extending the number of applications of SECM in electrocatalysis. Formic acid was generated at a Hg on Au ultramicroelectrode (UME) tip by reduction of CO2 in a 0.1 M KHCO3 solution saturated with this gas. The electrocatalytic activity of different Pd−Co bimetallic compositions was evaluated using a Pd−Co electrocatalyst array formed by spots deposited onto glassy carbon (GC) as a SECM substrate. The SECM tip, which generated a constant formic acid flux, was scanned above the array and the oxidation current generated when formic acid was collected by active electrocatalytic spots was displayed as a function of tip position. This generated a SECM image that showed the electrocatalytic activity of each spot. SECM screening identified Pd50Co50 (Pd/Co = 50:50, atomic ratio) as a better electrocatalyst toward the formic acid oxidation than pure Pd or Pt in 0.1 M KHCO3 solution and this result was confirmed by cyclic voltammetry. Positive feedback was observed for the most active compositions of Pd−Co which suggests fast reaction kinetics and chemical reversibility during the oxidation of formic acid to CO2. Moreover this feedback increases the contrast between active and non-active spots in this imaging mode.
ISSN:0003-2700
1520-6882
DOI:10.1021/ac901096h