The surfaces of fly ash (FA) particles were modified by surfactant, sodium lauryl sulphate (SLS) and used in fabrication of composite films with polyvinyl alcohol (PVA). Both unmodified fly ash (FA) and modified fly ash (SLS-FA) samples were examined using a range of analytical tools including X-ray fluorescence spectroscopy (XRF), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FTIR) and X-ray photoelectron spectroscopy (XPS). The distribution patterns of SLS-FA particles were shifted to the higher regions compared to FA by adding 1.2-4.2 ?m in the ranges between 2 and 25 ?m, whereas the modification process reduced the size of the particles over 25 ?m due to grinding during the activation process. The increased 1.2-4.2 ?m in average can be considered the thickness of the surfactant on the SLS-FA surface. On the oxides based chemical analysis by XRF, the compositions were almost unchanged. SEM and TEM were visualised the irregular sizes morphology mostly spherical of the particles, although it is impossible to capture the images of exactly same particles in modified and unmodified forms. The composite films reinforced with SLS-FA showed 33 higher strength than those of FA filled films. The enhancement of tensile strength attributed from the level of physical bonding between SLS-FA and PVA surfaces.