Thermal and thermomechanical properties of volcanic ash (VA) filled polyphenylene sulfide (PPS) composites were investigated with respect to silane treatment of VA and heat treatment of VA/PPS composites by differential scanning calorimeter (DSC) and dynamic mechanical thermal analysis (DMTA), respectively. The content of pristine VA was varied as 0, 5, 10, 15, 20, and 25 wt%. After determining the optimum VA contents (10 and 15 wt%), silane treatment was performed with 3-aminopropyltriethoxysilane (3-APTS). At last, PPS composites with pristine-and silane-treated VA particles with optimum contents were heat treated at 2008C for 2 h. Adhesion behavior between VA and PPS was examined by scanning electron microscopy (SEM). It was reported that thermal behavior of VA/PPS composites was dominantly affected by PPS instead of VAs. However, a direct linear relationship was found between the content of pristine VA and stiffness according to glassy storage modulus (E 0 ) and damping factor (tan d) results. It was determined that both silane and heat treatment had no significant effect on thermal properties. After silane treatment, a positive effect on both storage modulus and loss factor was obtained. Additionally, heat treatment caused significantly further positive effect on stiffness but drastically caused negative effect on damping. POLYM. COMPOS.,