Crystalline palladium–cobalt alloy nanoassemblies with enhanced activity and stability for the formic acid oxidation reaction

In this work, we conveniently synthesize the three-dimensionally (3D) networks-like palladium–cobalt alloy nanoassemblies (Pd–Co ANAs) through a simple simultaneous reduction reaction with sodium borohydride using inorganic K2PdCl4/K3Co(CN)6 cyanogel as reaction precursors, and clarify the formation mechanism of 3D networks structure and generation mechanism of Pd–Co alloy at room temperature. The morphology, structure, size and composition of the Pd–Co ANAs are characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), energy dispersive spectrum (EDS), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). Cyclic voltammetry, chronoamperometry and CO-stripping voltammetry tests demonstrate the Pd–Co ANAs have higher electrocatalytic activity, better electrochemical stability, and higher resistance to CO poisoning over single-component Pd nanoparticles for the formic acid oxidation reaction (FAOR) owing to their unique 3D structure and alloy property.

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► Pd–Co alloy nanoassemblies (Pd–Co ANAs) are obtained by cyanogel reduction.
► Pd–Co ANAs have particular 3D structure, abundant defects and high alloying degree.
► Pd–Co ANAs exhibit enhanced stability and activity for the formic acid oxidation.