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A NiCo2S4@PPy series with sheet stacking structure and suitable pore size distribution is successfully synthesized through a one‐step vulcanization process and polymerization process. Interestingly, the abundant sites and large electroactive surface area of NiCo2S4@PPy stacking structure are formed via the “etching effect” of S2− ions and ultrasonic oscillation effect, which render the morphology of NiCo2S4@PPy with a lamellar feature. In contrast, polypyrrole (PPy) with good conductivity provides favorable electron transport pathways for electrolyte ions. The as‐prepared sheet stacking structure NiCo2S4@PPy (NCSP‐3) electrode delivers good electrochemical properties with the highest specific capacitance of 1606.6 F g−1 at 1 A g−1 and excellent rate performance of 77.4% at high discharge rate of 10 A g−1. Furthermore, the NCSP‐3 electrode exhibits remarkable cycling stability, where the ultimate specific capacitance has no attenuation (retained at around 100%) compared with its incipient value after 20 000 cycles even at 20 A g−1. These promising results can be put down to the unique structure and synergetic effect of NiCo2S4 and PPy, which ensure good conductivity, more redox reactions, as well as large specific surface area. This work has guiding significance for the general and low‐cost route design of high‐performance electrode materials for supercapacitor applications.

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Designing electrode materials with high reversible capacitance is the key to developing high‐performance pseudocapacitors. In this work, a novel ternary hybrid material, porous ZnS@Co3S4@NiO nanosheets are successfully constructed through a morphology reshaping enabled by a hydrothermal method followed by calcination. From a macroscopic view, the introduction of NiO changes the nanorod morphology of ZnS@Co3S4, and forms a porous nanosheet structure. The porous architecture with an increased specific surface area can promote the transport of ions and electrons, accelerate the diffusion of the electrolyte, and offer more active sites for electrochemical reactions. These advantages enhance the electrochemical properties of ZnS@Co3S4@NiO nanosheets when used as electrode materials for supercapacitors. ZnS@Co3S4@NiO nanosheets deliver an initial capacitance of 1418.7 F g−1, and it also reaches 1550.9 F g−1 with a capacitance retention rate of 109.3% at 5 A g−1, after 5000 cycles. However, ZnS@Co3S4 nanorods only deliver an initial capacitance of 708.7 F g−1, and maintain 716.4 F g−1 with a capacitance retention rate of 101.1% after 5000 cycles. These results show that the ZnS@Co3S4@NiO nanosheets are a promising electrode material for high‐performance pseudocapacitor electrode, and morphology reshaping is an effective strategy to design high‐performance pseudocapacitive materials.