A novel synthetic route has been developed to prepare $alpha$-cobalt hydroxide with intercalated nitrate anions. It was successfully synthesized by $gamma$-ray irradiation under simple conditions, i.e., air atmosphere, without base. Under $gamma$-ray irradiation, it leads to the formation of layered cobalt hydroxynitrate compounds which have small crystalline size and have the role of a generator of hydroxyl anion. Structural and morphological characterizations were performed by using power X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and high resolution transmission electron microscopy (HR-TEM). The component and thermal stability of the sample were respectively measured by Fourier transform infrared (FT-IR) spectroscopy, elemental analysis, and thermal analyses, including thermogravimetry (TG) and differential thermal analysis (DTA).