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Polyacrylonitrile (PAN)/Fe2O3 nanocomposite membranes with a thickness of 0.02 mm were electrospun by adding 0 to 5 wt% of Fe2O3 into PAN. The surface tension, density, kinematic viscosity and dynamic viscosity of the PAN solution were determined to be 33.8±1 mN/m, 0.9794 g/ml, 1548.6 mm2/sec and 1516.7 cP, respectively. The average diameters of PAN fibers containing 0, 1, 2, 3, and 4 wt% Fe2O3 particles were 300, 260, 210, 130, and 90 nm, respectively. Fourier-transform infrared spectroscopy results showed that the addition of Fe2O3 nanoparticles to the PAN mat reduced the absorption peak intensity at 2242 cm−1 (C≡N bond) while it caused a sharp increase in the peak intensity at 2356 cm−1 (C=O bond). Thus, it appears that an appropriate amount of Fe2O3 nanoparticles in the PAN backbone leads to an improvement of the performance of the CO2 gas sensor, most likely due to the change of functional groups in the membrane.