Optimization of electrode preparation conditions by response surface methodology for improved formic acid electrooxidation on Pd/MWCNT/GCE

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Ulaş B.

Ionics, vol.29, no.11, pp.4603-4616, 2023 (SCI-Expanded) identifier

  • Publication Type: Article / Article
  • Volume: 29 Issue: 11
  • Publication Date: 2023
  • Doi Number: 10.1007/s11581-023-05171-z
  • Journal Name: Ionics
  • Journal Indexes: Science Citation Index Expanded (SCI-EXPANDED), Scopus, Chemical Abstracts Core, Compendex, INSPEC
  • Page Numbers: pp.4603-4616
  • Keywords: Electrode preparation, Formic acid electrooxidation, Multiwall carbon nanotube, Palladium, Response surface method
  • Van Yüzüncü Yıl University Affiliated: Yes


This work examines the formic acid electrooxidation capabilities of Pd catalysts supported by multiwall carbon nanotubes that were synthesized at varying weight percentages. Advanced surface analysis techniques, namely, X-ray diffraction, X-ray photoelectron spectroscopy (XPS), transmission electron microscopy, scanning electron microscopy with X-ray energy dispersive, and elemental mapping, are used to evaluate the Pd/MWCNT. To achieve the highest specific activity for formic acid electrooxidation on Pd/MWCNT, electrode preparation parameters, namely, catalyst slurry amount, ultrasonication duration of catalyst slurry, and electrode drying time, were optimized by response surface methodology-central composite design. Measurements made using cyclic voltammetry, electrochemical impedance spectroscopy, and chronoamperometry are used to determine the specific activity and stability of formic acid electrooxidation. The optimum values for the catalyst slurry amount, electrode drying time, and ultrasonication duration of catalyst slurry were determined as 1.84 μl, 45 min, and 37.05 min, while under these optimum conditions, the specific activity on Pd/MWCNT was 2.67 mA cm−2 with a deviation of 6.83%. By optimizing the electrode preparation conditions, a conventional Pd/MWCNT catalyst showed higher performance than many bimetallic catalysts. Optimization of electrode preparation parameters is as important as catalyst design and is an inexpensive and facile method to improve electrocatalytic performance. Graphical Abstract: [Figure not available: see fulltext.].