In this paper, nanoparticles of copper–cobalt compound oxide have been prepared by the sol–gel technique with different mole ratios of Cu/Co (ranging from 0.05 to 0.15) for the detection of methane gas, which is chemically a very stable hydrocarbon. The structural properties and morphology of the powders were studied by x-ray diffraction (XRD), Fourier transform infrared spectroscopy and transmission electron microscopy (TEM). By XRD analysis, we confirm that Co3O4 and (CuO0.3CoO0.7) Co2O4 phases are formed and mean grain size is decreased with increasing Cu doping (from 28 to 24 nm). On the basis of TEM images, it is found that these particles possess a cubic structure with nearly uniform distribution. Also, gas-sensing measurements reveal that the optimal operating temperature is 300 C, that the use of Cu as a dopant improved the sensing properties of cobalt oxide and that the sensitivity increased considerably with Cu concentration. The best sensitivity properties of nanosensors have been found at the mole ratios of Cu/Co of 0.125 and 0.15.

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