Ni-doped ZnO hollow microspheres were fabricated by calcining the mixture of zinc and nickel citrate precursors at 500 °C for 2 h. The structure, composition, Barrett–Emmett–Teller specific surface area, and optical properties of Ni-doped ZnO samples were characterized by x-ray diffraction, x-ray photoelectron spectroscopy, wave length dispersive x-ray fluorescence spectroscopy, field emission scanning electron microscopy, high-resolution transmission electron microscopy, N2 adsorption–desorption isotherms, and ultraviolet (UV)-visible diffuse reflectance spectroscopy. The photocatalytic results demonstrated that the as-synthesized Ni-doped ZnO microcrystals possessed much higher photocatalytic activity than pure ZnO in the decomposition of methylene blue under UV-light irradiation. The present work suggests that Ni-doped ZnO hollow microspheres can be applied as an efficient photocatalyst for water polluted by some chemically stable azo dyes.
