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

Abstract

This work examines the formic acid electrooxidation (FAEO) capabilities of Pd catalysts supported by multiwall carbon nanotubes (MWCNTs) that were synthesized at varying weight percentages. Advanced surface analysis techniques namely X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy with X-ray energy dispersive (SEM-EDX), and elemental mapping are used to evaluate the Pd/MWCNT. To achieve the highest speci c activity for FAEO on Pd/MWCNT, electrode preparation parameters namely catalyst slurry amount (V s ), ultrasonication duration of catalyst slurry (t u ), and electrode drying time (t d ) were optimized by response surface methodology central composite design (RSM-CCD). Measurements made using cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and chronoamperometry (CA) are used to determine the speci c activity and stability for FAEO. The optimum values for the V s , t d, and t u were determined as 1.84 µl, 45 min, and 37.05 min while under these optimum conditions, the speci c activity for FAEO 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. HighlightsPd/MWCNT/GCE electrode is developed for the FAEO.Response surface methodology is applied for optimum Pd/MWCNT/GCE preparation conditions. Pd/MWCNT/GCE has 2.67 mA cm -2 speci c activity for FAEO under optimum conditions.

Fabrication and Characterization of an Electrochemical Platform for Formaldehyde Oxidation, Based on Glassy Carbon Modified with Multi-Walled Carbon Nanotubes and Electrochemically Generated Palladium Nanoparticles

“…To date, the modification of CNTs with PdNPs to obtain a CNT/PdNP composite has been achieved through various methods, including chemical reduction of Pd(II) ions with sodium borohydride [13,53], formaldehyde [52,54], and sodium citrate in an ethylene glycol solution [55]. Other techniques involve the thermal decomposition of palladium acetate [39], RF magnetron sputtering [56], and electrochemical reduction of the MWCNT/lignosulfonate-Pd 2+ composite [57].…”