In this study, poly(vinyl alcohol) (PVA) nanocomposite fiber mats with sepiolite were prepared via electrospinning technique. The measurements of fourier transform infrared (FTIR) spectroscopy, differential scanning calorimetry (DSC), contact angle, scanning electron microscopy (SEM), and atomic force microscopy (AFM) were used for the characterization. The effect of polymer/sepiolite ratio and heat treatment on the properties of samples was investigated. The heat treatment which decreased the solubility of nanofibers and the addition of sepiolite resulted in a decrease in nanofiber diameter, contact angle with water, and water drop spreading rate on the material, and also resulted in an increase in water drop spreading rate inside the material. POLYM. COMPOS., 36:2334–2342, 2015. © 2014 Society of Plastics Engineers