A superelastic aerogel with fast shape recovery performance from large compressive strain is highly desired for numerous applications such as thermal insulation in clothing, high-sensitive sensors, and oil contaminant removal. Fabrication of superelastic cellulose nanofibrils (CNF) aerogels is challenging as the CNF can assemble into non-elastic sheet-like cell walls. Here, a dual ice-templating assembly (DITA) strategy is proposed that can control the assembly of CNF into sub-micrometer fibers by extremely low temperature freezing (-196 °C), which can further assemble into an elastic aerogel with interconnected sub-micron fibers by freezer freezing (−20 °C) and freeze drying. The CNF aerogel from the DITA process demonstrates isotropic superelastic behavior that can recover from over 80% compressive strain along both longitudinal and cross-sectional directions, even in an extremely cold liquid nitrogen environment. The elastic CNF aerogel can be easily modified by chemical vapor deposition of organosilane, demonstrating superhydrophobicity (164° water contact angle), high liquid absorption (489 g g −1 of chloroform absorption capacity), self-cleaning, thermal insulating (0.023 W (mK) −1 ), and infrared shielding properties. This new DITA strategy provides a facile design of superelastic aerogels from bio-based nanomaterials, and the derived high performance multifunctional elastic aerogel is expected to be useful for a wide-range of applications.
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