Controlled Formation of Polyimide Aerogel Networks in Carbon Fiber Felt via Multicycle Freeze-Drying for Thermal Protection.

Fiber-reinforced aerogel composites are attractive for thermal protection applications because porous polymer networks can suppress heat transfer while maintaining structural stability. In this study, carbon fiber felt was integrated with a polyimide aerogel via a freeze-drying-assisted multicycle impregnation process to achieve controlled formation of interconnected aerogel networks within the fibrous scaffold. With increasing impregnation cycles, the composites exhibited progressive microstructural densification and improved structural stability. Although bulk density increased, thermal protection performance under prolonged butane-torch exposure was significantly enhanced, showing delayed backside temperature rise and improved resistance to structural degradation compared with bare carbon felt. Post-ablation analyses revealed the formation of a micro-/nanoporous polymer-derived char layer and a multilayer thermal-resistance structure, which contributed to suppressed heat transfer during flame exposure. These results indicate that effective thermal protection in CF/PA composites is governed by dynamic microstructural evolution and char-layer formation rather than intrinsic room-temperature thermal conductivity alone. The proposed multicycle impregnation strategy provides a scalable approach for designing lightweight polymer-based thermal protection materials operating in high-temperature environments.