Nickel hydroxide nanosheets, nanobelts and nanorods were prepared by hydrothermal treatment of the precipitates obtained at different pH values. The morphology and crystal structure of the products could be controlled simply by adjusting the pH value at precipitation. Interconnected nanosheets of hexagonal β-Ni(OH) 2 with thickness around 10–20nm were formed at pH∼11, whereas nanobelts with typical widths around 40–80nm, and nanorods with diameters around 50–60nm of phase pure α-Ni(OH) 2 containing intercalated sulphate ions were obtained in the pH range ∼9.5–8.5. Thermal annealing of the hydroxides at 500°C yielded cubic phase NiO with morphologies similar to their hydroxide precursors. X-ray powder diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), and energy dispersive X-ray (EDX) analysis were used to characterize the as-prepared products. The role of pH in controlling the phase and morphology of the products was discussed.