Fast, Low‐Cost, and Lyophilization‐Free Synthesis of Multifunctional Elastic Nanofiber Aerogels

Abstract Aerogels are regarded as ideal materials across a range of fields due to their exceptionally low densities and highly porous structures. However, their practical applications are significantly constrained by their inherent fragility, high production costs, and demanding conditions such as freeze‐drying or supercritical drying. In this study, a novel, low‐cost strategy is presented for the large‐scale fabrication of hierarchically structured nanofiber aerogels (HENAs) using a lyophilization‐free, dissolution‐induced coordination (DIC) method. This approach enables fabrication within ≈4 h, which is 10 times faster than conventional lyophilization processes (usually require ≥48 h). Despite the absence of additional chemical crosslinking, the formation of stable coordination networks imparts the aerogels with excellent resilience (exhibiting only 3.9% deformation after 100 compression cycles). This strategy demonstrates fiber‐type invariant universality, enabling the fabrication of HENAs with multifunctional properties, including noise absorption (noise reduction coefficient of 0.58), electromagnetic wave absorption (effective absorption bandwidth of 7.2 GHz), and oil adsorption (adsorbing capacity of 36.4 g g −1 ). The simplicity, rapidity, and cost‐effectiveness of this synthesis approach provide a promising pathway for the large‐scale production of multifunctional aerogels.