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The bottom\u2010up on\u2010surface synthesis approach in ultra\u2010high vacuum allows for the synthesis of atomically well\u2010defined graphene or biphenylene nanoribbons and nanoporous graphene (NPG) structures suitable for device applications. Here, a novel 2D carbon allotrope is synthesized in the form of a functional NPG with periodically spaced biphenylene segments. First, 12\u2010armchair porous graphene nanoribbons (12\u2010pGNRs) on Au(111) and Au(788) using 7,10\u2010dibromo\u20101,4\u2010diphenyl\u2010triphenylene (DBDT) molecular precursor are grown. Low\u2010temperature scanning tunneling microscopy\/spectroscopy (LT\u2010STM\/STS) and non\u2010contact atomic force microscopy (nc\u2010AFM) measurements reveal the presence of high\u2010quality semiconducting 12\u2010pGNRs. Thermal annealing of densely packed 12\u2010pGNRs at 550\u00a0\u00b0C triggers their lateral fusion into diverse NPG structures featuring either graphene\u2010type or biphenylene\u2010type junctions. The structural and electronic properties are again characterized by LT\u2010STM and nc\u2010AFM in combination with density functional theory (DFT) calculations. DFT shows that while graphene\u2010type NPGs are direct bandgap semiconductors, biphenylene\u2010type NPGs manifest a smaller and indirect bandgap. The NPGs are stable upon oxygen and air exposure, and the nanopores feature a noticeable affinity to carbon monoxide, making them appealing systems for chemical sensors.<\/jats:p>","DOI":"10.1002\/adma.202511706","type":"journal-article","created":{"date-parts":[[2025,12,3]],"date-time":"2025-12-03T07:40:58Z","timestamp":1764747658000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":3,"title":["A Functional 2D Carbon Allotrope Combining Nanoporous Graphene and Biphenylene Segments"],"prefix":"10.1002","volume":"38","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-1770-0025","authenticated-orcid":false,"given":"Paula","family":"Angulo\u2010Portugal","sequence":"first","affiliation":[{"name":"Centro de F\u00edsica de Materiales (CFM\u2010MPC) CSIC\u2010UPV\/EHU  Manuel Lardizabal 5 San Sebastian 20018 Spain"},{"name":"Department of Polymers and Advanced Materials: Physics, Chemistry and Technology Faculty of Chemistry University of the Basque Country UPV\/EHU  San Sebastian 20018 Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3057-8076","authenticated-orcid":false,"given":"Martin","family":"Irizar","sequence":"additional","affiliation":[{"name":"Department of Polymers and Advanced Materials: Physics, Chemistry and Technology Faculty of Chemistry University of the Basque Country UPV\/EHU  San Sebastian 20018 Spain"},{"name":"Donostia International Physics Center (DIPC)  Manuel de Lardizabal 4 San Sebastian E\u201020018 Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Longfeng","family":"Huang","sequence":"additional","affiliation":[{"name":"Physics Department E20 TUM School of Natural Sciences Technical University of Munich  James\u2010Franck\u2010Stra\u00dfe 1 D\u201085748 Garching Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-1541-7066","authenticated-orcid":false,"given":"Mamun","family":"Sarker","sequence":"additional","affiliation":[{"name":"Department of Chemistry and Nebraska Center for Materials and Nanoscience University of Nebraska \u2212 Lincoln  Lincoln Nebraska 68588 USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Mustafa A.","family":"Ashoush","sequence":"additional","affiliation":[{"name":"Physics Department Faculty of Science Al\u2010Azhar University  Nasr City Cairo E\u201011884 Egypt"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-2385-7704","authenticated-orcid":false,"given":"Zakaria M. 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