Organic additives are widely used in the deposition baths of metals and alloys thanks to their special function which affects the growth and the building of the crystal. This study investigates the effect of glycerol on Ni deposition onto carbon felt (CF) and its effect on the catalytic activity towards glycerol electrooxidation. The impact of glycerol on the morphology, distribution, and particle size of the electrodeposited Ni is disclosed using a scanning electron microscope (SEM). X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and cyclic voltammetry (CV) techniques were used to probe the possible changes of the electrodeposited Ni oxide phases. Electrochemical measurements show that the as-synthesized Ni0.05@CF electrocatalyst prepared in the presence of 50 mM glycerol has a marked activity towards glycerol electrooxidation, as confirmed by the impressive increase of the oxidation current by about 1.6 times concurrently with a favorable negative shift of its onset potential. Moreover, the charge transfer resistance (R ct) is much reduced from 140 to 87 ohm. The addition of glycerol to the deposition bath is believed to retard the growth of the formed Ni deposits while enhancing the nucleation rate and thus increases the particle density and, consequently, the distribution of deposited Ni over the entire CF is improved along with increasing the surface concentration and surface-active sites. This assumption is supported by density functional theory (DFT) calculations.
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