Zinc hydroxide nitrate, an anionic exchanger layered material, undoped as well as doped with 2–10% nickel, was synthesized by using a pH-controlled precipitation method. The layered materials were then used to produce the undoped and nickel-doped zinc oxides by hydrothermal-treatment. X-ray diffraction, Fourier transform infrared spectroscopy and scanning electron microscopy confirmed the formation of pure phase undoped and nickel-doped layered materials, as well as the products of the hydrothermaltreated materials, nanostructured zinc oxides. Optical studies of the nanostructured zinc oxides showed a decrease in band gap with increasing content of the doping agent, nickel.
