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Herein, a general and scalable protocol is reported to prepare ultralight and robust pure COF fiber aerogels (FAGs), based on the epitaxial growth synergistic assembly (EGSA) strategy. Specifically, intertwined COF nanofibers (100\u2013200\u00a0nm) are grown in situ on electrospinning polyacrylonitrile (PAN) microfibers (\u22481.7\u00a0\u00b5m) containing urea\u2010based linkers, followed by PAN removal via solvent extraction to obtain the hollow COF microfibers. The resultant COF FAGs possess ultralow density (14.1\u201315.5\u00a0mg cm<jats:sup>\u22123<\/jats:sup>) and hierarchical porosity that features both micro\u2010, meso\u2010, and macropores. Significantly, the unique interconnected structure composed of nanofibers and hollow microfibers endows the COF FAGs with unprecedented mechanical properties, which can fully recover at 50% strain and be compressed for 20 cycles with less than 5% stress degradation. Moreover, the aerogels exhibit excellent capacity for organic solvent absorption (e.g., chloroform uptake of &gt;90\u00a0g g<jats:sup>\u22121<\/jats:sup>). This study opens new avenues for the design and fabrication of macroscopic COFs with excellent properties.<\/jats:p>","DOI":"10.1002\/smll.202311881","type":"journal-article","created":{"date-parts":[[2024,2,19]],"date-time":"2024-02-19T13:47:16Z","timestamp":1708350436000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":18,"title":["Ultralight and Robust Covalent Organic Framework Fiber Aerogels"],"prefix":"10.1002","volume":"20","author":[{"given":"Chengming","family":"Xiao","sequence":"first","affiliation":[{"name":"Key Laboratory of New Membrane Materials Ministry of Industry and Information Technology School of Environmental and Biological Engineering Nanjing University of Science and Technology Nanjing 210094 P. R. China"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Yiyuan","family":"Yao","sequence":"additional","affiliation":[{"name":"Key Laboratory of New Membrane Materials Ministry of Industry and Information Technology School of Environmental and Biological Engineering Nanjing University of Science and Technology Nanjing 210094 P. R. China"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Xin","family":"Guo","sequence":"additional","affiliation":[{"name":"Key Laboratory of New Membrane Materials Ministry of Industry and Information Technology School of Environmental and Biological Engineering Nanjing University of Science and Technology Nanjing 210094 P. R. 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