Surface analysis of nickel nanomaterials electrodeposited on graphite surface

Pure Nickel (Ni) and Nickel–Palladium (Ni–Pd) alloy were electrodeposited on graphite surface via pulse electrolysis in dimethyl sulfoxide in form of rods and nanoparticles with a diameter of ∼100–350 and ∼10–35 nm, respectively. X‐ray photoelectron spectroscopy (XPS) spectra of Ni 2p 3/2 region for these nanomaterials suggests on their surface Ni 2+ precursor while after Ar + ion‐etching metallic nickel starts to be dominated. Both Pd 0 and Pd 2+ for XPS spectra of Pd 3d 5/2 and 3d 3/2 were observed after electrodeposition. Scanning electron microscope‐energy dispersive X‐ray and XPS analysis confirmed electrodeposition of nickel nanomaterials in non‐aqueous electrolyte. Using a lower concentration of Ni 2+ precursor, nanoparticles with an average particle size of ∼10–23 nm were prepared on a graphite surface.