Effect of Annealing on Surface Morphology and Structure of Nickel Coatings Deposited from Deep Eutectic Solvents

Nanocrystalline nickel coatings deposited on a copper base material from DES made of choline chloride and ethylene glycol in 1:2 molar ratio containing 1 mol dm−3 NiCl2⋅6H2O were modified through post-deposition heat treatment at the temperatures from 100 to 400 °C. As-deposited coatings were composed of spheroidal agglomerates with the size of several hundred nanometers interspersed with lamellar crystals, but after annealing at 300 °C and 400 °C only single nano-sized plates embedded in a granular and porous layer remained. As the temperature of the heat treatment increased from 100 °C to 400 °C, the mean crystallite size increased from 13 to 35 nm. The change in crystallite size was accompanied by a change in microhardness, the maximum value of which was measured for the annealed coating at 200 °C. As a result of heat treatment, coatings were gradually covered by a layer of oxidized nickel species. XPS analyses showed that NiOOH and Ni(OH)2 dominated among them. Above 200 °C the share of these compounds began to decline in the face of the increasing share of NiO. This, in turn, clearly translated into a deterioration of the corrosion resistance of Ni coatings annealed at 300 °C, and especially at 400 °C, during exposure in 0.05 mol dm−3 NaCl solution.