Aqueous nanosilica sol (particle size range: 9-13 nm, pH: 9.0) was added at various low concentration range (0.5-2 wt.%) into aqueous poly (vinyl alcohol) (PVA) of different molecular weight (98% hydrolyzed, 20 wt.%) (pH: 5.0) at room temperature under constant stirring to synthesize organic-inorganic hybrid hydrogels in presence of sodium lauryl sulphate as a silica dispersant. Buffer tablets were added to arrest the pH at 9.0 (to prevent any silica aggregation due to change in pH). The resultant hybrids were cast on Teflon sheets and dried in an oven at 50°C to drive out all the unbound water. Those films were then subjected to freese-thaw treatment continuously for 5 h. The freese-thawed films appeared opaque. The swelling-de swelling experiments with the hydrogels were carried out in distilled water at room temperature and consequently allowed to de-swell naturally. Those observations were correlated with the microstructures of the hybrid hydrogels. © 2011 World Scientific Publishing Company.