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This approach achieves controlled symmetry breaking with precise polar group distribution, without the lattice disruption caused by asymmetric monomers in one\u2010pot methods. The resulting randomly oriented polar nanoregions exhibit relaxation behavior, collectively generating a strong piezoelectric response under external stimuli. Piezoresponse force microscopy (PFM) measurements indicate that TFB\u2010TAPT\u2010FA has a piezoelectric coefficient of 140 pm\/V, 2.5 times that of TFB\u2010TAPT. This amplification of the electromechanical response arises from the polar nanoregions, as evidenced by its higher calculated dipole moment (5.68 Debye). Consequently, TFB\u2010TAPT\u2010FA achieves an impressive piezocatalytic hydrogen production rate of 3.8 mmol g\n                    <jats:sup>\u22121<\/jats:sup>\n                    h\n                    <jats:sup>\u22121<\/jats:sup>\n                    , marking a 17\u2010fold improvement over TFB\u2010TAPT. Notably, TFB\u2010TAPT\u2010FA enables efficient hydrogen production without cocatalysts or heterojunctions. More broadly, the introduction of polar nanoregions similarly enhances the performance of other imine\u2010linked COFs, demonstrating a potentially general strategy for designing piezocatalysts through nanoscale polarization engineering in COFs.\n                  <\/jats:p>","DOI":"10.1002\/anie.3994811","type":"journal-article","created":{"date-parts":[[2026,10,13]],"date-time":"2026-10-13T06:09:09Z","timestamp":1791871749000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":1,"title":["Engineering Polar Nanoregions in COFs via Controlled Symmetry Breaking Toward Piezocatalysis"],"prefix":"10.1002","author":[{"given":"Ge","family":"Yan","sequence":"first","affiliation":[{"name":"Institute of Clean Energy Chemistry Key Laboratory for Green Synthesis and Preparative Chemistry of Adv. Mater. 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