Abstract3D‐networked, ultrathin, and porous Ni3S2/CoNi2S4 on Ni foam (NF) is successfully designed and synthesized by a simple sulfidation process from 3D Ni–Co precursors. Interestingly, the edge site‐enriched Ni3S2/CoNi2S4/NF 3D‐network is realized by the etching‐like effect of S2− ions, which made the surfaces of Ni3S2/CoNi2S4/NF with a ridge‐like feature. The intriguing structural/compositional/componental advantages endow 3D‐networked‐free‐standing Ni3S2/CoNi2S4/NF electrodes better electrochemical performance with specific capacitance of 2435 F g−1 at a current density of 2 A g−1 and an excellent rate capability of 80% at 20 A g−1. The corresponding asymmetric supercapacitor achieves a high energy density of 40.0 W h kg−1 at an superhigh power density of 17.3 kW kg−1, excellent specific capacitance (175 F g−1 at 1A g−1), and electrochemical cycling stability (92.8% retention after 6000 cycles) with Ni3S2/CoNi2S4/NF as the positive electrode and activated carbon/NF as the negative electrode. Moreover, the temperature dependences of cyclic voltammetry curve polarization and specific capacitances are carefully investigated, and become more obvious and higher, respectively, with the increase of test temperature. These can be attributed to the components' synergetic effect assuring rich redox reactions, high conductivity as well as highly porous but robust architectures. This work provides a general, low‐cost route to produce high performance electrode materials for portable supercapacitor applications on a large scale.

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The intrinsic zinc dendrite growth aggravated by the uneven electric field at the Zn anode surface and the water‐induced parasitic reactions have largely impeded rechargeable aqueous zinc‐ion batteries for the practical applications in large‐scale energy storage. Here, an effective strategy is proposed to manipulate Zn deposition and simultaneously prevent the generation of insulating by‐products (Zn4SO4(OH)6·xH2O) for improved plating/stripping on Zn anodes by the addition of a nontoxic electrolyte additive, β‐cyclodextrin (β‐CD). The simulation results indicate that β‐CD molecules prefer to adsorb horizontally on Zn (002) plane, regulating the diffusion pathways and deposition sites of Zn2+ for the preferred Zn deposition along (002) plane without dendrite formation and inhibiting the H2 generation and the formation of Zn4SO4(OH)6·xH2O by facilitating desolvation of [Zn(H2O)6]2+. Consequently, an ultra‐long stable cycling up to 1700 h at a high current density of 4 mA cm−2 can be achieved by the addition of β‐CD, 17 times that of the pure ZnSO4 electrolyte and the remarkable stability is also maintained under harsh test condition (40 mA cm−2, 20 mAh cm−2). This study highlights the important role of β‐CD in engineering the interfacial stability during Zn plating/stripping for high‐performing aqueous batteries.

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