Nanobelts of nickel hydroxyl sulfate have been prepared on a large scale via a simple template-free hydrothermal reaction on the basis of a complex [Ni(NH(3))(6)](2+) formed with Ni(2+) and ammonia in an ethanol-water solution. The as-synthesized nanobelts were single crystals, with several tens of microns in length and 50-150 nm in width. The nanobelts were enclosed by top surfaces (100) and side surfaces (001) and their growth direction was parallel to [010]. The function of aqueous ammonia and ethanol was discussed. Furthermore, nanostructures of a mixture of crystralline NiO and amorphous nickel sulfate with various morphologies, such as nanobelts, porous nanobelts, and nanoparticles, were obtained by the thermal treatment of the as-synthesized Ni(SO(4))(0.3)(OH)(1.4) nanobelts at different temperatures.