In this paper, three-dimensional carbon superstructures (CSSs) have been proposed through an effective method. Specifically, the hierarchical self-assembly of polyimide (PI) is followed by thermal annealing. Moreover, the structural evolution of PI under the various pyrolysis time was also comprehensively studied. It is noted that the as-prepared CSSs as anode composites for LIBs, especially CSS-5 h, exhibited extraordinary electrochemical properties, exhibiting a high reversible performance, great rate performance, and excellent cycling stability. As expected, the superior electrochemical capability can be ascribed to the synergistic effect of combining the nanoflower-like carbon superstructures with nitrogen contents. Such a method might encourage the inspirations to devise and obtain various heteroatom-modulated and hierarchical polymer-derived carbon composites for LIBs.
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