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The hurdle of fabricating asymmetric supercapacitor (ASC) devices using a faradic cathode and a double layer anode is challenging due to the required large amount of active mass of anodic material compared to that of the cathodic material during mass balancing due to the large difference in capacitance values of the two electrodes. Here, the problem is addressed by engineering a negative electrode that furnishes an ultrahigh capacitance. An in situ developed metal–organic framework (MOF)‐based thermal treatment is adopted to grow highly porous N‐doped carbon nanotubes (CNTs) containing submerged Co nanoparticles over nano‐fibrillated electrospun hollow carbon nanofibers (HCNFs). The optimized CNT@HCNF‐1.5 furnishes an ultrahigh capacitance approaching 712 F g–1 with excellent rate capability. The capacitance reported from this work is the highest for any carbonaceous material reported to date. The CNT@HCNF‐1.5 is further used to fabricate symmetric supercapacitors (SSCs), as well as ASC devices. Remarkably, both the SSC and ASC devices furnish incredible performances in all aspects of SCs, such as a high energy density, long cycle life, and high rate capability, displaying decent practical applicability. The energy density of the SSC device reaches as high as 20.13 W h kg–1, whereas that of ASC approaches 87.5 W h kg–1. An in situ developed metal–organic framework‐based thermal treatment technique is adopted to prepare porous N‐doped carbon nanotubes containing firmly submerged Co‐nanoparticles over nano‐fibrillated electrospun hollow carbon nanofibers. When the optimized CNT@HCNF‐1.5 is applied as a negative electrode, the problem related to mass balancing during fabrication of asymmetric supercapacitor can be addressed satisfactorily that will open new possibilities for the future works.

The development of smart negative electrode materials with high capacitance for the uses in supercapacitors remains challenging. Although several types of electrode materials with high capacitance in energy storage have been reported, carbon-based materials are the most reliable electrodes due to their high conductivity, high power density, and excellent stability. The most common complaint about general carbon materials is that these electrode materials can hardly ever be used as free-standing electrodes. Free-standing carbon-based electrodes are in high demand and are a passionate topic of energy storage research. Electrospun nanofibers are a potential candidate to fill this gap. However, the as-spun carbon nanofibers (ECNFs) have low capacitance and low energy density on their own. To overcome the limitations of pure CNFs, increasing surface area, heteroatom doping and metal doping have been chosen. In this review, we introduce the negative electrode materials that have been developed so far. Moreover, this review focuses on the advances of electrospun nanofiber-based negative electrode materials and their limitations. We put forth a future perspective on how these limitations can be overcome to meet the demands of next-generation smart devices.