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The initial stages of Zn–Ni electrodeposition have been investigated through a study of composition and structure of thin deposits on copper and iron substrates. Compositional gradients through the 0.05 μm thick deposits formed at 10 and 60 mA cm −2 have been obtained using Glow Discharge Optical Emission Spectrometry (GDOES) and Scanning Transmission Electron Microscopy (STEM). The results...