Direct electroreduction of solid cuprous chloride to prepare copper powder in a"neutral"ambient-temperature ionic liquid,1-butyl-3-methylimidazolium tetrafluoroborate ionic liquid(BMIMBF4)was investigated.Cyclic voltammetry of the CuCl powder in a Pt-powder cavity microelectrode exhibited that solid CuCl can be electrochemical reduced in the ionic liquid.Chronoamperometry of the salt powder filled Mo-cavity electrode(current collector)in the ionic liquid further demonstrated the conversion of chloride to metal inside the cavity,as confirmed by scanning electron microscopy,energy-dispersive X-ray,and X-ray diffraction spectra.
The electrodeposition behaviors of nickel on glassy carbon（GC） and carbon steel（CS） electrodes were investigated in the14.3%-85.7%（mole fraction） betaine.HCl ethylene glycol（EG） ionic liquid using cyclic voltammetry and chronoamperometry.The results indicated that the reduction of Ni（Ⅱ） on CS electrode via a diffusion-controlled quasi-reversible process was much more facile and easier than that occurred on GC electrode,which followed a diffusion-controlled three-dimensional instantaneous nucleation and growth.Scanning electron microscopy was used to observe that the deposit was dense and contained fine crystallites with average size of（80±4） nm.Energy dispersive spectrometer analysis showed that the obtained deposit was metallic nickel.X-ray diffraction spectroscopy indicated that（111） plane was the most preferred crystal orientation.The nickel deposit was luminous and bright,and had good adhesion with the CS substrate.
The electrodeposition behavior of nickel at glassy carbon(GC)and stainless steel(SS)electrodes in low temperature urea-acetamide-NaBr-KBr melt was investigated using cyclic voltammetry,chrono-amperometric current-time transients and scanning electron microscopy.Cyclic voltammograms and dimensionless chronoamperometric current-time transients analysis show that the electrodeposition of nickel is an irreversible process and proceeds via three-dimensional progressive nucleation with diffusion-controlled growth on both GC and SS substrates.Scanning electron microscopic analysis indicates the nickel deposits obtained on SS electrode are generally uniform,dense,and adherent to the substrate with rounded crystallites in the nanometer size regime.It is also found that the crystal structure of the electrodeposited nickel is independent on the deposition potential.The nickel deposits produced from the melt at higher cathodic potential exhibit larger grain size.
