Flower-shaped β- Ni(OH) 2 structures composed of thin nanosheet networks have been synthesized via the simple aqueous solution route by using nickel chloride and ammonium hydroxide at 65 ∘ C in 4 h. The general morphological observations revealed that the flowers are composed of thin nanosheets which were connected to each other in such a manner that they form network-like morphologies. Moreover, single-crystalline flower-shaped NiO structures composed of thin nanosheets were also obtained by thermal decomposition of flower-shaped β- Ni(OH) 2 structures. The shape of nanosheet networks in β- Ni(OH) 2 was sustained after thermal decomposition to NiO however, some broken nanosheets were also observed from the flower-shaped structures of NiO. The as-prepared products were characterized by X-ray powder diffraction (XRD), field emission scanning electron microscope (FESEM), transmission electron microscope (TEM), high-resolution TEM (HRTEM), Fourier transform infrared spectroscopy (FTIR), and Thermogravimetric analysis (TGA).