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2D MXene materials have attracted intensive attention in energy storage application. However, MXene usually undergoes serious face‐to‐face restacking and inferior stability, significantly preventing its further commercial application. Herein, to suppress the oxidation and self‐restacking of MXene, an efficient and fast self‐assembly route to prepare a 3D porous oxidation‐resistant MXene/graphene (PMG) composite with the assistance of an in situ sacrificial metallic zinc template is demonstrated. The self‐assembled 3D porous architecture can effectively prevent the oxidation of MXene layers with no evident variation in electrical conductivity in air at room temperature after two months, guaranteeing outstanding electrical conductivity and abundant electrochemical active sites accessible to electrolyte ions. Consequently, the PMG‐5 electrode possesses a striking specific capacitance of 393 F g−1, superb rate performance (32.7% at 10 V s−1), and outstanding cycling stability. Furthermore, the as‐assembled asymmetric supercapacitor possesses a pronounced energy density of 50.8 Wh kg−1 and remarkable cycling stability with a 4.3% deterioration of specific capacitance after 10 000 cycles. This work paves a new avenue to solve the two long‐standing significant challenges of MXene in the future. [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]