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SYNOPSISPolyimide-silica hybrid materials were prepared by polycondensation, polyimidization, and sol-gel coreactions. Several aminoalkoxysilane precursors providing a chemical bonding between the inorganic and the organic phase were used. During the synthesis, the molecular structure of the materials prepared with these precursors were followed at various steps by 29Si-NMR (nuclear magnetic resonance). The final materials were characterized at the macroscopic level by thermogravimetric analysis and scanning electron microscopy and at the molecular level by infrared spectrometry and 29Si-MAS-NMR spectroscopy. It has been demonstrated that the properties of the organic sidegroups of the bonding agent are determinent on the properties of the final material.