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As promising candidates for widespread application, advanced ceramic fiber mats with robust mechanical properties are urgently needed. However, the brittleness, fatigue failure, and large density of ceramic fiber pose significant obstacles to its practical application. Herein, a novel SiO2 aerogel/ZrO2 composite nanofibrous membrane (SZCNFM) with excellent flexibility was prepared by introducing SiO2 aerogel nanoparticles into ZrO2 nanofiber via simple co‐electrospinning. The developed tetragonal zirconia phase without changing up to 1200°C endows SZCNFM material with excellent thermal stability. Furthermore, the as‐prepared membranes exhibit fatigue resistance ability which can maintain 98% of the original stress after 100 buckling cycle tests. The addition of mesoporous structure aerogel reduces the heat transfer of the nanofibrous membrane, giving its low thermal conductivity (30 mW/m/K) and low‐frequency sound absorption (noise reduction coefficient of 0.52). Combined with the high‐temperature resistance, low thermal conductivity and excellent sound‐absorption ability make it a promising material for heat insulation and acoustic absorption. [ABSTRACT FROM AUTHOR]

Nanofibrous aerogel composites have emerged as most promising materials for their high-temperature insulation in complex environments due to their ultra lightweight, high elasticity, and superior thermal performance. However, the release of particles caused by weak bond strength between nanofibers and aerogel, lead to insulation failure which presents serious challenge. This research presents, a novel approach to mitigate the particle release and significantly improve the overall performance of nanofibrous aerogel composites. The proposed method involves the preparation of particle-free nanofibrous aerogel composites through unique combination of sol-aerogel blending, electrospinning, and freeze-casting processes. The effect of particle release has been successfully eliminated by embedding TiO 2 aerogel within SiO 2 nanofibers even under rigorous conditions (weight loss rate less than 0.57%). Furthermore, the resulting nanofibrous aerogel composite exhibits exceptional thermal insulation properties, with a low thermal conductivity of 0.0251 W/mK at room temperature. Additionally, the proposed composite material configuration demonstrates superior infrared radiation suppression performance resulting in an infrared transmittance of 39.52%. The lamellar structure of the nanofibers aerogel is tailored to provide high compressive strength (2.2 kPa at 40% strain), exceptional cyclic fatigue resistance after 50 cycles, and temperature (−196 to 500 °C) conditions. The outstanding combination of thermal and mechanical properties exhibited by these nanofibrous aerogel composites makes them highly promising for stable thermal protection in extreme environmental conditions. These novel materials promise great potential for application in various engineering industries where reliable thermal insulation is critical. [ABSTRACT FROM AUTHOR]