ABSTRACT As the velocity of aerospace vehicles increases and the service environment of thermal protection systems (TPS) becomes more severe, there is an urgent need to develop lightweight materials that are resistant to ablation in oxidizing atmospheres over extended periods. This study employs a sol–gel method combined with atmospheric pressure drying (APD) to incorporate dimethoxymethylphenylsilane (DMMPS) and the silane coupling agent 3‐isocyanatopropyltrimethoxysilane (IPTS) for preparing a