The roles of zinc and nitrate ions in the electrochemical growth of ZnO were examined in this study. ZnO was deposited on a polycrystalline Cu substrate from electrolyte containing 0.0025–0.08 M zinc nitrate and 0.1–2.0 M potassium nitrate. The morphology, epitaxial orientation relationship, interfacial microstructure, and photoluminescence (PL) properties of the ZnO deposits were characterized. The ZnO morphology was found to be controlled mostly by the zinc ion concentration in the electrolyte. Here, 50–400 nm wide hexagonal pillars were deposited from electrolyte with potassium nitrate concentration as high as 0.4 M. All the deposited films had strong 〈0001〉//ND fibre texture. Most of the ZnO crystallites were grown epitaxially on Cu grains regardless of the electrolyte concentration. The major epitaxial orientation relationship was identified as (0001)ZnO//(103)Cu and [11
2
¯
0]ZnO//[010]Cu, and three other epitaxial orientation relationships were also identified. Samples consisting of nanopillars or plates exhibited excellent PL characteristics with near bandgap–deep level emission intensity ratios of 2.4–4.3 and full width at half maximum of the NBE peak of 122–131 meV.
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