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Its distinctive structural feature is the presence of sp\u2010hybridized carbon atoms, which endow GDY with unique properties, including natural bandgap, high porosity, large specific surface area, expanded interlayer spacing, high electrical conductivity, and excellent charge carrier mobility. Achieving high crystallinity and precise thickness control is essential for unlocking the intrinsic properties of GDY. However, the irreversibility of the HEB polymerization reaction, along with side reactions and the free rotation of Csp\u2010Csp and Csp\n                    <jats:sup>2<\/jats:sup>\n                    \u2010Csp single bonds, limits the crystallinity of GDY. Meanwhile, axial growth induced by interlayer van der Waals forces and \u03c0\u2010\u03c0 stacking complicates thickness control. The review summarizes controllable synthesis methods for monolayer, few\u2010layer, and multilayer GDY, as well as recent experimental advances in understanding the structural and electronic properties of GDY. It further extends to the synthesis of crystalline GDY derivatives, aiming to provide a solid theoretical and technical foundation for large\u2010scale synthesis of crystalline and ultrathin GDY in the future.\n                  <\/jats:p>","DOI":"10.1002\/smll.75737","type":"journal-article","created":{"date-parts":[[2026,9,23]],"date-time":"2026-09-23T09:56:26Z","timestamp":1790157386000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Controllable Synthesis of Crystalline 2D Graphdiyne With Tunable Thickness"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0009-0008-6058-6820","authenticated-orcid":false,"given":"Guilin","family":"Hu","sequence":"first","affiliation":[{"name":"Chongqing Key Laboratory of Green Synthesis and Applications College of Chemistry and Materials Science Chongqing Normal University  Chongqing P. R. 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