Hybrid organic-inorganic membranes were fabricated using sol-gel technique using PMMA and TEOS with 80/20 (w/w) ratio at various solvents. The thin membrane films were then characterized using DSC and TGA. From DSC analysis, the Tg value of the PMMA moieties in hybrids membranes was in the order H-15-Toluene < Pure PMMA < H-15-THF < H-15-DMF. Furthermore, from TGA analysis it was found that the hybrid membranes have higher thermal stability compared to pure PMMA, and the type of solvents used play an important role in their degradation behavior.