Abstract

AbstractLow density (≤13.9 mg cm−3), compressible poly(bis(benzimidazo)benzophenanthroline‐dione) (BBB) sponges with high temperature resistance are reported. The processing of BBB is limited due to its insolubility in organic solvents and infusibility. Therefore, the sponges are made in two steps: first, the BBB fibers are prepared by electrospinning the starting monomers with a template polymer followed by polycondensation of monomers on solid fibers at high temperature. In the second step, the BBB fibers are mechanically cut and self‐assembled from a dispersion during freeze‐drying. The use of poly(vinyl alcohol) is critical in getting self‐assembled hierarchically double‐pore‐structured, mechanically stable sponges. The sponges show very high pyrolytic stability, high compressibility (more than 92% recovery after 50% compression), very low thermal conductivity (0.028–0.038 W mK−1), and high oil absorption capacity.

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