We report the preparation of flexible polystyrene/polypyrrole (PS/PPy) mats and their successful use as a resistive humidity sensor. These composite membranes were prepared by first obtaining PS films through the electrospinning technique, and then incorporating PPy chains by an in situ chemical polymerization of the pyrrole monomer. The PS fibers were homogeneously distributed, with diameters that obeyed a normal distribution with an average value of (1.04 ± 0.12) μm. The deposition of conducting PPy chains on the surface of the PS fibers was confirmed after characterizing the PS/PPy mats by Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), contact angle measurements, and electrochemical impedance spectroscopy (EIS). When used as humidity sensors, the PS/PPy mats exhibited a sensor response of 128.6%, with fast response ((54.9 ± 3.5)s) and recovery times ((76.8 ± 11.1)s), and stable response under different humidity conditions over several days. These performance characteristics compare favorably to those of previous resistive humidity sensors discussed in the literature.
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