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Here, we report a synthesis strategy that breaks this constraint by employing self-assembled ABC triblock terpolymer base materials with a gyroid nanoarchitecture and one cross-linked end block as robust 3D templates for the spatially defined in-gel functionalization of the tethered non-cross-linked blocks. We demonstrate this generalizable concept with selective amine attachment in the C end block for selective metal ion coordination, uptake, and nanostructure-directed metal nanoparticle synthesis. Additionally, phase-confined sulfonation is achieved selectively on both the middle B and end C blocks, respectively, producing, to the best of our knowledge, the first monolithic gyroidal hydrogels exhibiting tunable swelling up to 600 vol % and nanoconfined hydration while maintaining structural integrity. Combined sequential and block-selective functionalization generates a nanostructured, pH-responsive polyampholyte material bearing blocked cationic and anionic polymer chains tethered to the continuous and cross-linked gyroidal network. The achieved decoupling of structural and chemical versatility in these cross-linked BCP gels provides a modular platform and design paradigm for studying nanoconfined synthesis, nanoarchitected ion-exchange membranes, and stimuli-responsive smart materials.<\/jats:p>","DOI":"10.1021\/jacs.6c09785","type":"journal-article","created":{"date-parts":[[2026,9,29]],"date-time":"2026-09-29T14:02:10Z","timestamp":1790690530000},"page":"43050-43060","source":"Crossref","is-referenced-by-count":0,"title":["Spatially Defined Chemical\nFunctionalization of Ordered\nBlock Copolymer Materials"],"prefix":"10.1021","volume":"148","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-7569-2887","authenticated-orcid":true,"given":"Yuanzhi","family":"Li","sequence":"first","affiliation":[{"name":"Boston University , , 110 Cummington Mall , , ,","place":["Boston, Massachusetts, United States, 02215"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-2383-4476","authenticated-orcid":true,"given":"Sarah A.","family":"Hesse","sequence":"additional","affiliation":[{"name":"SLAC National Accelerator Laboratory , , , ,","place":["Menlo Park, California, United States, 94025"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Wenlu","family":"Wang","sequence":"additional","affiliation":[{"name":"Boston University , , 15 St. Mary\u2019s Street , , ,","place":["Boston, Massachusetts, United States, 02215"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7845-086X","authenticated-orcid":true,"given":"Jo\u0308rg G.","family":"Werner","sequence":"additional","affiliation":[{"name":"Boston University , , 110 Cummington Mall , , ,","place":["Boston, Massachusetts, United States, 02215"]},{"name":"Boston University , , 15 St. Mary\u2019s Street , , ,","place":["Boston, Massachusetts, United States, 02215"]},{"name":"Boston University , , 590 Commonwealth Ave , , ,","place":["Boston, Massachusetts, United States, 02215"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,9,29]]},"reference":[{"issue":"6","key":"2026101414073306900_cit1","doi-asserted-by":"publisher","first-page":"1602","DOI":"10.1021\/ma60078a047","article-title":"Theory of\nMicrophase Separation in Block Copolymers","volume":"13","author":"Leibler","year":"1980","journal-title":"Macromolecules"},{"issue":"1","key":"2026101414073306900_cit2","doi-asserted-by":"publisher","first-page":"525","DOI":"10.1146\/annurev.pc.41.100190.002521","article-title":"Block Copolymer\nThermodynamics: Theory and Experiment","volume":"41","author":"Bates","year":"1990","journal-title":"Annu.\nRev. 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