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As a recently emerging group of 2D materials, MXene has attracted extensive attention in the energy storage field in recent years owing to their outstanding features. However, the notorious issues of inevitable oxidation stability and surface‐to‐surface self‐restacking for MXene significantly prevent its further wide‐ranging application. Herein, the 3D macroporous oxidation‐resistant Ti3C2Tx MXene/graphene/carbon nanotube (MRC) hybrid hydrogels are prepared by a simple gelation method assisted by l‐cysteine as crosslinker and l‐ascorbic acid (VC) as reductant. Benefitting from the effectively alleviated restacking, excellent electrical conductivity, and the 3D inter‐crosslinked macroporous architecture, as a supercapacitor electrode, the obtained MRC aerogel exhibits a superior specific capacitance of 349 F g−1, unparalleled rate capability (52.0% at 3000 mV s−1) and amazing cyclic stability (retention of 97.1% after 100 000 cycles). Moreover, the 3D MRC‐30 aerogel exhibits an impressive oxidation‐resistant performance with just a 9.3% increase in electrical resistance after storing in ambient condition for 60 days, effectively alleviating the oxidation problem of MXene. This work demonstrates a new method for construction of 3D oxidation‐resistant MXene hydrogel, shedding new light on the promising applications of MXene materials, especially in high humidity and oxygen environment. [ABSTRACT FROM AUTHOR]

Potassium‐ion hybrid capacitors have attracted increasing attention due to good energy density, high power density, and low cost. Ti3C2Tx‐MXene is considered as a promising anode material for K ion storage. However, undesirable stacking issues decrease its exposed area and breeds sluggish K ion transport. Herein, a facile spray‐lyophilization strategy is proposed to construct stacking‐resistant Ti3C2Tx with 3D structures. As‐prepared Ti3C2Tx hollow spheres/tubes present stack resistance, a large specific surface area, and a short ion diffusion pathway. When serving as an anode material, it shows enhanced capacity and thickness‐independent rate performance compared to 2D Ti3C2Tx. After 10 000 cycles, a specific capacity of 122 mAh g−1 is obtained at 1 A g−1. Systematic kinetics analyses demonstrate the significance of concentration polarization on the electrode's rate ability. Furthermore, a 3D Ti3C2Tx‖hierarchical porous activated carbon (HPAC) K‐ion hybrid capacitor is assembled and displays remarkable energy and power densities with energy retention of 100% after 10 000 cycles at 1 A g−1. Following this strategy, other 3D structures from nanosheets can also be obtained, such as 3D Ti3C2Tx microtubes and graphene oxide nanoscrolls. This study provides a viable approach to solve the stacking issues of 2D nanosheets to promote the application of 2D materials. [ABSTRACT FROM AUTHOR]