Urchin-like Ni O superstructures have been prepared via a thermal decomposition reaction of Ni C2O4 at 400 for 1h. The morphology and structure of the synthesized urchin-like superstructures have been characterized by X-ray diffraction, field emission scanning electron microscopy and transmission electron microscopy. The results show that urchin-like Ni O superstructures were a polycrystal with cubic structure and typical diameters of 200 to 500 nm and the self-assembly nanoparticles average diameter is 14 nm. The as-prepared Ni O superstructures have a high Brunauer-Emmett-Teller surface area of about 60.32 m2/g. The UV-vis spectrum of urchin-like Ni O consists of one peak at 357 nm（3.47 e V）.
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