Polymers reinforced with metal oxide nanoparticles exhibit interesting possibilities from application point of view due to homogeneous distribution of nanoparticles, and superior thermal and mechanical properties. In the present work, SiO2, ZrO2 and ZnO nanoparticles were prepared by the microwave hydrothermal method, and nanocomposites based on them were processed in polyvinyl alcohol (PVA) matrix. The thermal decomposition behaviour of pure PVA and composites was studied using the thermal gravimetric analysis (TGA) and differential scanning calorimetry (DSC). In the case, of composites, at 50% weight loss, the temperature was shifted by nearly 80°C, in comparison to the pure PVA. The SiO2 doped nanocomposites showed, a three stage temperature decomposition in the DSC spectra.