Influence of additives and pulse electrodeposition parameters on production of nanocrystalline zinc from zinc chloride electrolytes

Pulse electrodeposition was used to produce nanocrystalline zinc from an aqueous zinc chloride electrolyte with polyacrylamide and thiourea as additives. The influence of additive concentration and pulse electrodeposition parameters, namely, current-on time, current-off time, and peak current density on the grain size, surface morphology, and preferred orientation was investigated. The grain size and surface morphology of zinc deposits were studied by scanning electron microscopy and field emission scanning electron microscopy. The preferred orientation of zinc deposits was studied by X-ray diffraction. The optimum concentrations of polyacrylamide and thiourea in the bath that give the finest grains were 0.7 and 0.05 g/L, respectively. At constant current-off time and peak current density, the grain size decreased asymptotically with increasing current-on time. An increase in the current-off time at constant current-on time and peak current density resulted in grain growth. A progressive decrease of the grain size was observed with increasing peak current density at constant current-on and -off time. Nanocrystalline zinc with an average grain size of 50 nm was obtained at a peak current density of 1000 mA/cm2. The crystal orientations developed were correlated to the variation in the cathode overpotential accompanied with changing the electrodeposition parameters. A (1013) preferred orientation was developed at low overpotential while higher overpotential developed a dual (1122) (1010) orientation.