Homogeneous cellulose/silica gel polymer hybrids were prepared by hydrolysis of acetyl cellulose (AcCL) in a sol-gel reaction mixture of alkoxysilane such as tetramethoxysilane (TMOS). To a mixture of AcCL and TMOS in a mixed solvent of THF and methanol (v/v, 7/3), an HCl aqueous solution was added to initiate hydrolysis and condensation of the alkoxysilane. The resulting mixture was constantly stirred for 5 h and heated at 60 A degrees C for two weeks to allow evaporation of the solvents. Consequently, corresponding transparent and homogeneous polymer hybrids could be obtained in a range of mass ratios (AcCL/TMOS = 1/5-1/2). In the FT-IR spectra, the absorption peaks corresponding to the acetyl group decreased as the amount of 0.1 M aqueous HCl solution increased, which indicates hydrolysis of acetyl groups of AcCL, whereas the intensity of the Si-O-Si stretching vibration peak increased. The thermal properties of the obtained polymer hybrids were evaluated by TG/DTA and DSC measurements.