This research work presents the fabrication of polyaniline (PANI) and graphene–polyaniline (graphene–PANI) nanocomposite-coated polystyrene (PS) nanofibre mats, as well as their application in flexible and highly sensitive gas sensors. The surface morphology of the flexible films is investigated using a number of techniques. The profilometry studies confirmed that the electrospun fibres are evenly distributed over a large surface area and there was no visible difference between coated and uncoated fibres. The SEM morphology studies revealed that a nanocomposite consisting of 10 nm PANI nanofibres and graphene forms a uniform coating around 3 μm diameter PS fiber. AFM showed differences in the 3D surface topography between plain PS nanofibres and coated ones, which showed an increased roughness. Moreover, conductive AFM has indicated an increase in the electrical current distribution from picoamperes to nanoamperes of the PS samples coated with PANI and graphene–PANI because of the applied voltage to the AFM tip that contacted the sample surface. The chemical properties of all the samples are analysed by Fourier transform infrared spectroscopy (FTIR) and X-ray powder diffraction (XRD), which revealed the presence of chemical interactions between the nanocomposites and the polymeric backbones. The TGA study indicated that graphene–PANI coated fibres have the highest thermal stability compared to the pure fibres. The addition of the nanocomposite layer to the PS fibre significantly increased the electrical conductivity. Therefore, nanocomposite-coated flexible membranes are used to fabricate carbon dioxide gas sensors (sensing range: 20–100 ppm). Due to the higher surface area of the nanocomposite coated fibre the availability of adsorption area is also higher, which leads to an increase in sensitivity to carbon dioxide gas. The sensitivity increases with the increase in gas concentration. The average response time of the sensor is calculated to be 65 seconds, with good and uniform repeatability.
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