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Here, hydrophobic microphase separation is identified as a microenvironmental mechanism governing CPDs formation. CPDs are proved to possess a hydrophobic core and a hydrophilic shell, consistent with nanoscopic domains of reduced water accessibility during hydrothermal growth. These hydrophobic microphases locally shift reversible dehydration equilibria toward water loss, particularly dehydrative condensation, thereby sustaining polycondensation, crosslinking, and carbonization. The resulting microphase\u2010promoted dehydration process drives the nucleation and growth of CPDs. By independently tuning monomer hydrophobicity and crosslinking confinement, mechanism\u2010guided regulation of CPDs size and product fraction is achieved. These findings establish microphase\u2010promoted dehydration as a chemical principle for the rational hydrothermal synthesis of carbon nanomaterials.<\/jats:p>","DOI":"10.1002\/anie.7521352","type":"journal-article","created":{"date-parts":[[2026,10,5]],"date-time":"2026-10-05T14:43:24Z","timestamp":1791211404000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Hydrophobic Microphase Separation\u2010Driven Polycondensation and Carbonization for the Formation of Carbonized Polymer Dots"],"prefix":"10.1002","author":[{"given":"Xiao","family":"Han","sequence":"first","affiliation":[{"name":"State Key Laboratory of Supramolecular Structure and Materials College of Chemistry Jilin University  Changchun P. R. 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