Nanocrystalline nickel oxide (NiO) was deposited onto glass substrates using a chemical deposition method from a bath containing nickel (Ni2+) ions and urea at 363 K. The deposition process was based on the reaction between Ni2+ and hydroxide ions released from the protolysis of ammonia formed in the decomposition of urea heated at 363 K, which caused to form nickel hydroxide. The structural properties of nickel oxide films were studied by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM). The XRD analyses showed that nanocrystalline nature remained after heating at 523 K for 2 h. Surface morphology of the nickel oxide film showed worm-like mesoporous structure with pore size in a nanometer range. The chemically deposited nickel oxide films were effectively used as a liquefied petroleum gas (LPG) sensor and the maximum response of 36.5%was recorded on exposure to 0.3 vol%of LPG at 698 K.