Single-crystal cubic NiO nanorods with diameters of 30–80 nm and lengths of up to tens of micrometers were synthesized by using a simple precursor thermal decomposition in NaCl flux with NiCO 3 as the precursor, which was prepared by one-step, solid-state reaction of NiCl 2·6H 2O and Na 2CO 3 at ambient temperature. The crystallinity, purity, morphology, and structure features of the as prepared NiO nanorods were investigated by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), high-resolution transmission electron microscopy (HRTEM), and Raman spectrum.