In the present study, NiO nanoparticles with average particle size of 35 nm were successfully prepared by solvothermal method. Thecrystal microstructure,composition, morphologyand particle size distribution of product was analyzed by using X-ray diffraction (XRD),Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and EDAX. A sensor for detection of vapors of volatile organic compounds (VOCs) such as ethanol, isopropyl alcohol and acetone is tested using NiO nanoparticles. One of the key features of the sensor is the use of nanostructured NiO material which has been synthesized using a novel low cost process. Considerable reduction in the operating temperature of the sensor has been achieved by using nanostructured NiO material. The maximum sensitivity of sensor was observed for Ethanol. © 2015, Sphinx Knowledge House. All rights reserved.