Abstract

We report a paired electrolysis method to prepare graphite nanoflakes (GNFs) and their supported noble metal/alloy nanoparticles (NM NPs/GNFs), by applying an alternating voltage (AV) on two graphite rod electrodes in a NaOH solution without/with noble–metal ions. The synthesis of GNFs might be related to the anodic exfoliation of graphite surface via OH− intercalation, accompanying the dispersion effect of hydrogen/oxygen gases evolution. The preparation of NM NPs/GNFs should be resulted from repeated coupling processes, namely the cathodic deposition of NM NPs and the electrochemical exfoliation-dispersion of NM NPs-decorated graphite layer. The as-prepared products were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-disperse X-ray spectra (EDX), powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), atomic absorption spectroscopy (AAS) and inductively coupled plasma (ICP). The GNFs and NM NPs/GNFs exhibited high electrocatalytic activities toward the redox of 4-nitrophenol and oxidation of formic acid, respectively.

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