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Here, we report a green and rapid two-stage strategy for constructing UiO-66-NH2 self-assembled aerogels with a bimodal micro-\/mesoporous architecture. A brief thermal pretreatment (130 \u00b0C, 3 h) is used solely for precursor activation, after which the critical MOF crystallization and in situ self-assembly are driven under ambient conditions via ultrasonic cavitation (900 W, 15\u201360 min). This protocol simultaneously drives the nucleation, crystallization, and self-assembly of UiO-66-NH2 nanocrystals into a monolithic, self-supporting architecture, thereby replacing the conventional prolonged high-temperature solvothermal MOF crystallization with a rapid room-temperature process. The sonication time critically governs the structural evolution, transforming initially amorphous aggregates into well-defined regular octahedral nanocrystals that form an interconnected framework. The optimized aerogel (UNA-T60) exhibits an exceptional specific surface area (1196.9 m2 g\u22121) and a synergistic bimodal pore structure comprising intrinsic micropores and intercrystalline mesopores. This architecture enables rapid mass transfer and active-site accessibility, resulting in a maximum Congo Red (CR) adsorption capacity of 660.56 mg g\u22121, with kinetics conforming to the pseudo-second-order model (R2 &gt; 0.999). The robust monolithic structure endows the material with outstanding reusability, retaining 90.8% of its initial adsorption capacity after four regeneration cycles. This work presents a paradigm-shifting approach for the sustainable fabrication of pure MOF aerogels, offering a promising solution for advanced dye wastewater treatment.<\/jats:p>","DOI":"10.3390\/gels12090778","type":"journal-article","created":{"date-parts":[[2026,9,1]],"date-time":"2026-09-01T09:48:36Z","timestamp":1788256116000},"page":"778","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Ultrasound-Induced In Situ Self-Assembly of Bimodal Micro\/Mesoporous UiO-66-NH2 Aerogels for High-Performance Congo Red Capture"],"prefix":"10.3390","volume":"12","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-0745-1405","authenticated-orcid":false,"given":"Tian","family":"Zhao","sequence":"first","affiliation":[{"name":"School of Materials Science and Engineering, Hunan University of Technology, Zhuzhou 412007, China"}],"role":[{"vocabulary":"crossref","role":"author"},{"role":"conceptualization","vocabulary":"credit"},{"role":"methodology","vocabulary":"credit"},{"role":"funding-acquisition","vocabulary":"credit"},{"role":"writing-original-draft","vocabulary":"credit"},{"role":"writing-review-editing","vocabulary":"credit"}]},{"given":"Shilin","family":"Peng","sequence":"additional","affiliation":[{"name":"School of Materials Science and Engineering, Hunan University of Technology, Zhuzhou 412007, China"}],"role":[{"vocabulary":"crossref","role":"author"},{"role":"investigation","vocabulary":"credit"},{"role":"visualization","vocabulary":"credit"},{"role":"writing-original-draft","vocabulary":"credit"},{"role":"writing-review-editing","vocabulary":"credit"}]},{"given":"Yan","family":"Wu","sequence":"additional","affiliation":[{"name":"School of Materials Science and Engineering, Hunan University of Technology, Zhuzhou 412007, China"}],"role":[{"vocabulary":"crossref","role":"author"},{"role":"formal-analysis","vocabulary":"credit"},{"role":"investigation","vocabulary":"credit"}]},{"given":"Tianhang","family":"Wang","sequence":"additional","affiliation":[{"name":"School of Materials Science and Engineering, Hunan University of Technology, Zhuzhou 412007, China"}],"role":[{"vocabulary":"crossref","role":"author"},{"role":"formal-analysis","vocabulary":"credit"}]},{"given":"Xing","family":"Zhang","sequence":"additional","affiliation":[{"name":"School of Materials Science and Engineering, Hunan University of Technology, Zhuzhou 412007, China"}],"role":[{"vocabulary":"crossref","role":"author"},{"role":"formal-analysis","vocabulary":"credit"}]},{"given":"Zhuoheng","family":"Li","sequence":"additional","affiliation":[{"name":"School of Materials Science and Engineering, Hunan University of Technology, Zhuzhou 412007, China"}],"role":[{"vocabulary":"crossref","role":"author"},{"role":"investigation","vocabulary":"credit"}]},{"given":"Xiangjiang","family":"Wu","sequence":"additional","affiliation":[{"name":"School of Materials Science and Engineering, Hunan University of Technology, Zhuzhou 412007, China"}],"role":[{"vocabulary":"crossref","role":"author"},{"role":"investigation","vocabulary":"credit"}]},{"given":"Ying","family":"Chen","sequence":"additional","affiliation":[{"name":"School of Materials Science and Engineering, Hunan University of Technology, Zhuzhou 412007, China"}],"role":[{"vocabulary":"crossref","role":"author"},{"role":"formal-analysis","vocabulary":"credit"}]},{"ORCID":"https:\/\/orcid.org\/0009-0009-4499-0695","authenticated-orcid":false,"given":"Yi","family":"Chen","sequence":"additional","affiliation":[{"name":"School of Materials Science and Engineering, Hunan University of Technology, Zhuzhou 412007, China"}],"role":[{"vocabulary":"crossref","role":"author"},{"role":"resources","vocabulary":"credit"},{"role":"supervision","vocabulary":"credit"},{"role":"funding-acquisition","vocabulary":"credit"},{"role":"writing-review-editing","vocabulary":"credit"}]}],"member":"1968","published-online":{"date-parts":[[2026,8,31]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","first-page":"26401","DOI":"10.1007\/s13399-024-05941-3","article-title":"Synthesis of Zr-doped CeO2 nanoparticles for photocatalytic degradation of methyl orange and electrochemical properties","volume":"15","author":"Haribaaskar","year":"2025","journal-title":"Biomass Convers. 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