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Low-temperature assembly of MXene nanosheets into three-dimensional (3D) robust aerogels addresses the crucial stability concern of the nano-building blocks during the fabrication process, which is of key importance for transforming the fascinating properties at the nanoscale into the macroscopic scale for practical applications. Herein, suitable cross-linking agents (amino-propyltriethoxysilane, Mn 2+ , Fe 2+ , Zn 2+ , and Co 2+ ) as interfacial mediators to engineer the interlayer interactions are reported to realize the graphene oxide (GO)-assisted assembly of Ti 3 C 2 T  x   MXene aerogel at room temperature. This elaborate aerogel construction not only suppresses the oxidation degradation of Ti 3 C 2 T  x   but also generates porous aerogels with a high Ti 3 C 2 T  x   content (87 wt%) and robustness, thereby guaranteeing the functional accessibility of Ti 3 C 2 T  x   nanosheets and operational reliability as integrated functional materials. In combination with a further sulfur modification, the Ti 3 C 2 T  x   aerogel electrode shows promising electrochemical performances as the freestanding anode for sodium-ion storage. Even at an ultrahigh loading mass of 12.3 mg cm −2 , a pronounced areal capacity of 1.26 mAh cm −2  at a current density of 0.1 A g −1  has been achieved, which is of practical significance. This work conceptually suggests a new way to exert the utmost surface functionalities of MXenes in 3D monolithic form and can be an inspiring scaffold to promote the application of MXenes in different areas.

Room-Temperature Assembled MXene-Based Aerogels for High Mass-Loading Sodium-Ion Storage