Since the SARS-CoV-2 pandemic, the interest in applying nanofibers t air filtration and personal protective equipment has grown significantly. Due to their morphological and structural properties, nanofibers have potential applications for air filtration in masks and air filters. However, most nanofiber membrane materials used for these purposes are generally non-degradable materials, which can contribute to the disposal of plastic waste into the environment. Hence, this work aims to produce polyvinyl alcohol (PVA) and chitosan (CS) biodegradable nanofibers with controlled morphology and structure via electrospinning. An experimental design was used to investigate the effects of the PVA|CS ratio and concentration on the properties of the electrospinning compositions and electrospun nanofiber mat. The electrospinning parameters were constant for all experiments: Voltage of 20 kV, a feed rate of 0.5 mL·h−1, and a distance of 10 cm between the needle and a drum collector. CS proved to be an efficient adjuvant to the PVA's electrospinning, obtaining a wide range of nanofiber diameters. Furthermore, 6.0% PVA and 1% CS were the best compositions after optimization with the response surface methodology, with a mean fiber diameter of 204 nm. The addition of biocide agents using the optimized condition was also investigated, using surfactants, citric acid, and pure and encapsulated essential oils of Lippia sidoides. Pure oil improved the material without enlarging the nanofiber sizes compared to the other additives. The nanofiber membranes produced have the potential to be used in air filtration or wound-dressing applications where biocidal activity is needed. [ABSTRACT FROM AUTHOR]