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While molecular intercalation surpasses ionic methods in preserving the crystallinity and intrinsic properties of 2D materials, its broader adoption is limited by weak driving forces and slow kinetics. To address these challenges, we propose an interlayer modulation strategy using H\n                    <jats:sub>3<\/jats:sub>\n                    PO\n                    <jats:sub>4<\/jats:sub>\n                    \u2010amine complexes as mediators. Structural and molecular dynamics analyses demonstrate that these complexes regulate interlayer proton activity through strong hydrogen bonding, thereby optimizing interlayer dynamics to enable in situ PW\n                    <jats:sub>12<\/jats:sub>\n                    formation and efficient graphite exfoliation. The PW\n                    <jats:sub>12<\/jats:sub>\n                    intercalant shows excellent recyclability via simple alkaline hydrolysis and regeneration, establishing a sustainable route for graphene production. This work overcomes the barrier to molecular intercalation by rationally engineering complex molecular intercalation, achieving universal and high\u2010throughput exfoliation of van der Waals layered materials.\n                  <\/jats:p>","DOI":"10.1002\/smtd.202502143","type":"journal-article","created":{"date-parts":[[2026,1,14]],"date-time":"2026-01-14T09:18:56Z","timestamp":1768382336000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Engineering Complex Molecular Intercalation for Efficient, Sustainable Exfoliation of Van Der Waals Layered Materials"],"prefix":"10.1002","volume":"10","author":[{"given":"Zhengyu","family":"Wei","sequence":"first","affiliation":[{"name":"Department of Applied Chemistry School of Chemistry Xi'an Key Laboratory of Sustainable Energy Material Chemistry Xi'an Jiaotong University  Xi'an P. R. 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