In this paper, novel organic pollutants gas sensing material CuAlO2 microspheres constituted of nanopartides were successfully prepared by wet chemical route and characterized by structural (XRD, XAS), morphological (SEM, TEM, HRTEM) and thermal (TG) analysis. In addition, the oxidation (O-3 and NO2) and reduction (NH3 and CO) toxic gas sensing properties of the prepared CuAlO2 microspheres were systematically investigated. CuAlO2 microspheres exhibited real-time response for very low detection level of 200 ppb at 200 degrees C, with fast response (29 s), recovery (45 s) time, good reproducibility and stability to ozone gas indicating their promising application in toxic gas sensor which is better than other oxidation and reduction gases. Also comparative studies of charge-transport properties mainly ascribed to the increased proportion of ozone gas exposed surface active layers are discussed in gas sensing mechanism. (C) 2015 Elsevier B.V. All rights reserved.