The electrochemical behavior of Co(II) reduction and Co nucleation/growth process on glassy carbon (GC) electrode in 1-ethyl-3methylimidazolium bisulfate ([EMIM]HSO 4 ) ionic liquid (IL) and ethylene glycol (EG) system is investigated. Cyclic voltammetry (CV) measurements indicate that Co(II) reduction occurs by a one-step process, Co(II) to Co(0), and it is an irreversible reaction. The diffusion coefficient of Co(II) is 2.24 × 10 −6 cm 2 s −1 at 323 K in the system. Chronoamperometry measurements show that the growth/nucleation process of Co on GC electrode in [EMIM]HSO 4 -EG is a three-dimensional (3D) progressive nucleation at lower overpotentials and instantaneous nucleation at higher overpotentials under diffusion controlled growth process. These effects of electrodepositing potential, current density and temperature on Co coating thickness are also investigated. The Co coatings are observed by energy dispersive spectrometer (EDS), scanning electron microscope (SEM) and X-ray diffractometer (XRD). SEM micrographs confirm that the Co coatings are relatively loose with a fibrous surface morphology. XRD pattern of the prepared coating reveals the characteristic peak of crystalline Co with a preferred orientation direction and the average size of Co grains is 11 nm. The nanocrystalline Co coating exhibits an excellent catalytic activity and stability for hydrogen evolution reaction (HER) in alkaline medium.

The codeposition behavior of Co(II) and Ni(II) in 1-ethyl-3-methylimidazolium bisulfate ([EMIM]HSO 4 ) ionic liquid (IL) and ethylene glycol (EG) system is recorded using cyclic voltammetry (CV). The result indicates that the mechanism of Co-Ni codeposition is an anomalous codeposition, and both the inhibition for Ni(II) reduction and the anomalous codeposition phenomena can be improved by the increase of Co(II) concentration in the system. These Co-Ni deposits are characterized using EDS, XRD and SEM. SEM micrographs indicate that the surface morphology of Co-Ni deposits can be changed by the increase of Co content, and these deposits with many additional elongated acerose crystals, which are germinated on the spherical "nodules" surface, can be prepared. XRD pattern reveals the feature peak of crystalline Co 1.2 Ni 2.8 with a preferred orientation direction and the average size of grains is calculated to be about 14.6 nm. Moreover, the electrocatalytic activity for hydrogen evolution reaction (HER) on the prepared Co-Ni catalyst surface is investigated using linear sweep voltammetry (LSV) and electrochemical impedance spectra (EIS). These results indicate that the obtained catalyst presents an excellent electrocatalytic activity and durability for HER with an overpotential of 139 mV at 10 mA cm −2 in 1 M KOH solution.

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