Catalytic Activity Evaluation of the Molten Salt-Modified Novel Ni Electrodes for Urea Electrooxidation in Alkaline Solutions

The presented paper characterized the molten salt-modified Ni electrode with excellent catalytic activity towards alkaline urea electrooxidation reaction. The electrodes were modified by electrodeposition of Al from molten salt electrolytes containing NaCl-KCl-AlF3 at a temperature of 750 °C and applied potential of −1.9 V. The porous surface was obtained by anodic polarization with a potential of −0.4 V until the anodic current was equal to 0 mAcm−2. The prepared deposits’ structure, surface morphology, and composition were analyzed using scanning electron microscopy (SEM) and X-ray diffraction (XRD). Anodic polarization was applied to assess the electrocatalytic activity and elucidate the urea electrooxidation mechanism in 1 M KOH + 0.33 M urea solution. The nanocrystalline structure, fine grain size, and microcracks on the surface of the studied electrodes contributed to their notably high electrochemically active surface area (ECSA). The cyclic voltammetry in the non-Faradaic regions of the samples shows that molten salt modification can increase the double layer capacitance of bare Ni plates by around ten times, from 0.29 mFcm−2 to 2.16 mFcm−2. Polarization of the electrodes in urea-containing KOH solution with potential of +1.52 V shows a significant difference in catalytic performance. For the bare nickel sample, the registered current density from the urea electrooxidation reaction was around +1 mAcm−2, and for the molten salt-modified one, it was +38 mAcm−2, which indicates the fact that the molten salt surface treatment can be a promising tool in tailoring the electrochemical properties of materials.