In this study, cobalt oxide Co 3 O 4 nanostructured material is synthesized by hydrothermal method by using different concentration of cobalt acetate salt at unique hydrothermal reaction time for five different hydrothermal reaction temperatures 105, 120, 140, 160, and 180 C. The obtained nanoparticles are annealed at 300 C for 5 h. Co 3 O 4 nanostructures are determined by means of scanning electron microscopy (SEM), X-ray diffraction (XRD), and UV-vis spectroscopy. The hydrothermally produced samples were reannealed at 550 C, and morphological and structural properties were investigated deeply again. The effect of annealing temperature on morphologies and crystalline structure of cobalt oxide nanoparticle (NP) was also investigated. Nanopyramids and nanorods are two main morphologically obtained structures from the hydrothermal experiment. Nematic liquid crystal mixture E7 is doped with Co 3 O 4 nanorod. Phase transition and threshold voltage of pure and Co 3 O 4 NP-doped E7 LC are examined successfully. It reveals that for Co 3 O 4 NP-doped E7 phase transition temperature and threshold voltage increased very slightly.