Solution processed NiSe2 nanorods were synthesized by a modified colloidal synthesis technique, by chemical reaction of TOPSe and nickel acetate at 150 ∘C. The rods exist as an oleic acid ligand stabilized solution, with oleic acid acting as a capping group. Structural characterization by X-ray diffraction and transmission electron microscopy indicates that the particles are rod-like shaped crystals with a high and relatively constant aspect ratio (30 : 1). TEM shows that the width and the length of the nanorods are in the range 10–20nm and 300–350 nm, respectively. XRD indicates that the nanorods are pure and well crystallized. The size of nanorods based on the Debye-Scherrer effect, was 150 nm, the average value of length and width. They display thermal stability over prolonged heating times (<100 >hours) at 150 ∘C, for which the average particle size is roughly constant. After about 100 hours of heating time there is an onset and growth of micron sized cubes and concurrent decomposition of NiSe2 to Ni and NiSe at 150 ∘C.