Structured design helps to play out the coordination advantage and optimize the performance of electrochemical reactions. In this work, hierarchical hollow microspheres (Co₃S₄@NiCo₂S₄) with unique core-shell heterostructure were successfully prepared through simple template and solvothermal methods. Thanks to the hollow structure, cross-linked nanowire arrays, and in-situ coating of zeolite imidazole framework (ZIF), Co₃S₄@NiCo₂S₄ demonstrated excellent electrochemical performance with a specific capacitance of up to 2697.7 F g⁻¹ at 1 A g⁻¹ and cycling stability of 80.5% after 5000 cycles. The covalent organic framework (COF) derived nano carbon, which had undergone secondary calcination and ZnCl₂ activation, also exhibited excellent double-layer energy storage performance. Compared to a single calcination, the incredible increase in capacitance was up to 208.5 times greater, reaching 291.9 F g⁻¹ at 1 A g⁻¹ while maintaining ultra-high rate performance (81.0% at 20 A g⁻¹). The hybrid supercapacitor, assembled with Co₃S₄@NiCo₂S₄ as the cathode and COF-derived carbon as the anode, exhibited an extremely high energy density (79.7 Wh kg⁻¹ at 693.5 W kg⁻¹) and excellent cyclic stability (maintained 79.3% after 10,000 cycles of 20 A g⁻¹), further explaining the reliable and practical characteristics. This work provided reference for the structural optimization of transition metal sulfides and the high-temperature activation of COF-derived carbon.

结构化设计有助于发挥配位优势，优化电化学反应性能。在这项工作中，成功地制备了具有独特核壳异质结构的分层空心微球（Co ₃ S ₄ @NiCo ₂ S ₄ ）通过简单的模板法和溶剂热法制备。由于中空结构、交联纳米线阵列和沸石咪唑骨架（ZIF）的原位涂层，Co ₃ S ₄ @NiCo ₂ S ₄ 表现出优异的电化学性能，在1 A g ⁻¹ 时比电容高达2697.7 F g ⁻¹ ，5000次循环后循环稳定性为80.5%。经过二次煅烧和ZnCl ₂ 活化的共价有机骨架（COF）衍生的纳米碳也表现出优异的双层储能性能。与单次煅烧相比，电容令人难以置信地增加了 208.5 倍，在 1 A g ⁻¹ 时达到 291.9 F g ⁻¹ ，同时保持超高倍率性能 (81.0% 20 A g ⁻¹ ）。混合超级电容器，以 Co ₃ S ₄ @NiCo ₂ S ₄ 作为阴极，COF 衍生碳作为阳极组装而成，表现出极高的能量密度（693.5 W kg ⁻¹ 时为79.7 Wh kg ⁻¹ ）和出色的循环稳定性（20 A g ⁻¹ ），进一步阐释了可靠、实用的特点。该工作为过渡金属硫化物的结构优化和COF衍生碳的高温活化提供参考。