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X-ray activation overcomes the depth barrier, but an integrated platform that simultaneously addresses hypoxia and provides persistent afterglow feedback remains lacking. Herein, we report a self-sustaining afterglow scaffold (TBR) constructed from a triphenylamine-derived sulfur-containing heterocycle bearing a p-dimethylaminophenylvinyl terminal group, featuring a donor\u2212\u03c0\u2013donor\u2212\u03c0\u2013acceptor (D\u2212\u03c0\u2013D\u2212\u03c0\u2013A) architecture around an aggregation-induced emission core. After nanoprecipitation with Pluronic F127, TBR nanoparticles (TBR-NPs) adopt a fluorescence-quenched state enabled by an ultrasmall singlet\u2013triplet energy gap, thereby maximizing X-ray energy conversion to generate both oxygen-independent type-I (\u2022OH, O2\u2022\u2013) and type-II (1O2) reactive oxygen species (ROS). Critically, the initially generated ROS undergo cycloaddition with TBR to form a cyclic peroxide intermediate; spontaneous dark decomposition releases stored chemical energy, re-exciting adjacent TBR molecules to sustain ROS production and generate near-infrared afterglow via a chemically initiated electron exchange luminescence (CIEEL) mechanism. This self-sustaining loop enables fractionated X-ray regimens that yield higher cumulative ROS than continuous exposure, while the type-I pathway ensures efficacy under hypoxia. A tumor-activatable derivative (BTBR) with H2O2-responsive boronate caging achieves high-contrast, tumor-specific afterglow imaging (signal-to-background ratio &amp;gt; 120) and enables hypoxic tumor ablation (95.8% inhibition) with real-time afterglow monitoring. By establishing a unified molecular platform that overcomes the dual barriers of penetration depth and hypoxia, this work provides a robust and generalizable strategy for advancing X-ray-triggered afterglow imaging-guided cancer therapy.<\/jats:p>","DOI":"10.1021\/jacs.6c18200","type":"journal-article","created":{"date-parts":[[2026,10,9]],"date-time":"2026-10-09T11:02:39Z","timestamp":1791543759000},"page":"45216-45234","source":"Crossref","is-referenced-by-count":0,"title":["X-ray-Triggered\nSelf-Sustaining Afterglow Scaffolds\nwith Persistent Type-I\/II ROS Generation for Imaging-Guided Hypoxic\nTumor Therapy"],"prefix":"10.1021","volume":"148","author":[{"ORCID":"https:\/\/orcid.org\/0009-0005-9654-8867","authenticated-orcid":true,"given":"Qinghao","family":"Zhou","sequence":"first","affiliation":[{"name":"Xi\u2019an Jiaotong University , , ,","place":["Xi\u2019an, P.R. China, 710049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Junfei","family":"Song","sequence":"additional","affiliation":[{"name":"Xi\u2019an Jiaotong University , , ,","place":["Xi\u2019an, P.R. China, 710049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Cheng","family":"Li","sequence":"additional","affiliation":[{"name":"Xi\u2019an Jiaotong University , , , ,","place":["Xi\u2019an, Shaanxi, China, 710004"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Arsalan","family":"Raza","sequence":"additional","affiliation":[{"name":"University of Science and Technology of China , , , ,","place":["Hefei, Anhui, China, 230026"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Guopu","family":"Huang","sequence":"additional","affiliation":[{"name":"Xi\u2019an Jiaotong University , , ,","place":["Xi\u2019an, P.R. China, 710049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Youshen","family":"Wu","sequence":"additional","affiliation":[{"name":"Xi\u2019an Jiaotong University , , , ,","place":["Xi\u2019an, Shaanxi, China, 710049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7449-0936","authenticated-orcid":true,"given":"Khurshed","family":"Bozorov","sequence":"additional","affiliation":[{"name":"Samarkand State University , , University Blvd. 15 , ,","place":["Samarkand, Uzbekistan, 140104"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zhidong","family":"Wang","sequence":"additional","affiliation":[{"name":"Xi\u2019an Jiaotong University , , , ,","place":["Xi\u2019an, Shaanxi, China, 710004"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-2668-6974","authenticated-orcid":true,"given":"Zhishen","family":"Ge","sequence":"additional","affiliation":[{"name":"Xi\u2019an Jiaotong University , , ,","place":["Xi\u2019an, P.R. China, 710049"]},{"name":"Xi\u2019an Jiaotong University , , , ,","place":["Xi\u2019an, Shaanxi, China, 710004"]},{"name":"University of Science and Technology of China , , , ,","place":["Hefei, Anhui, China, 230026"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,10,9]]},"reference":[{"issue":"11","key":"2026102111085972400_cit1","doi-asserted-by":"publisher","first-page":"1102","DOI":"10.1038\/nbt.3987","article-title":"Molecular afterglow imaging with\nbright, biodegradable polymer nanoparticles","volume":"35","author":"Miao","year":"2017","journal-title":"Nat. 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Soc.\nRev."},{"issue":"22","key":"2026102111085972400_cit5","doi-asserted-by":"publisher","first-page":"10970","DOI":"10.1039\/D4CS00599F","article-title":"Light\/X-ray\/ultrasound activated\ndelayed photon emission of organic molecular probes for optical imaging:\nmechanisms, design strategies, and biomedical applications","volume":"53","author":"Qu","year":"2024","journal-title":"Chem. Soc. Rev."},{"issue":"22","key":"2026102111085972400_cit6","doi-asserted-by":"publisher","first-page":"11207","DOI":"10.1039\/D4CS00443D","article-title":"Reactive\noxygen species-mediated\norganic long-persistent luminophores light up biomedicine: from two-component\nseparated nano-systems to integrated uni-luminophores","volume":"53","author":"Li","year":"2024","journal-title":"Chem. Soc. 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