Copolymers with different weight ratios of AA/PAS (acrylic acid/poly(DL-aspartic acid)) were synthesized and blended with sol-gel precursors to prepare water-soluble PAA-PAS/SiO(2) inorganic/organic hybrid materials. The PAS polymer or its copolymer in PAA-PAS/SiO(2) formed hydrogen bonds with SiO(2) and the amorphous structure of the hybrid material varied with the weight ratio of PAA. The hybrid materials exhibited enhanced thermal resistance over the copolymer alone. All hybrid materials were water-soluble and relatively insoluble in organic solvents.