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In this work, both liquid-phase and gaseous products generated from HAN decomposition over Rh\/C catalysts were systematically investigated. For the first time, direct EPR and HRMS evidence confirmed the formation of hydroxyl (\u2022OH) and nitric oxide (NO\u2022) radicals in aqueous HAN solutions during Rh\/C-catalyzed decomposition. Mechanistic analysis suggested that nascent \u2022OH originated from the homolytic cleavage of HNO3, while NO\u2022 was subsequently generated through reactions between \u2022OH (or NO2\u2022) and NH3OH+. XPS characterization of both fresh and spent Rh\/C catalysts indicated that metallic Rh0 acted as the active site for HAN decomposition. In situ ATR-IR and Raman spectroscopy captured changes in the N\u2013O and N\u2013OH bonds of aqueous HAN during the reaction. This study provided unambiguous evidence for radical involvement in HAN decomposition and proposed a revised radical-involved reaction pathway. These findings advance the fundamental understanding of HAN catalysis and offer guidance for the optimization of HAN-based propulsion systems.<\/jats:p>","DOI":"10.1021\/acs.jpcc.6c04485","type":"journal-article","created":{"date-parts":[[2026,10,27]],"date-time":"2026-10-27T04:01:42Z","timestamp":1793073702000},"source":"Crossref","is-referenced-by-count":0,"title":["Detection and Origin\nof Radical Species in the Catalytic\nDecomposition of Hydroxylammonium Nitrate Aqueous Solution"],"prefix":"10.1021","author":[{"given":"Xing","family":"Zhang","sequence":"first","affiliation":[{"name":"Dalian Polytechnic University , , ,","place":["Dalian, P. R. China, 116034"]},{"name":"Chinese Academy of Sciences , , ,","place":["Dalian, P. R. China, 116023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Shu","family":"Liu","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Dalian, P. R. China, 116023"]},{"name":"University of Chinese Academy of Science , ,","place":["Beijing, P. R. China, 100049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ming","family":"Tian","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Dalian, P. R. China, 116023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yabin","family":"Wang","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Dalian, P. R. China, 116023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Baolin","family":"Hou","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Dalian, P. R. China, 116023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Qingda","family":"An","sequence":"additional","affiliation":[{"name":"Dalian Polytechnic University , , ,","place":["Dalian, P. R. China, 116034"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Guangyi","family":"Li","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Dalian, P. R. China, 116023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8705-1278","authenticated-orcid":true,"given":"Xiaodong","family":"Wang","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Dalian, P. R. China, 116023"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,10,27]]},"reference":[{"issue":"3","key":"2026102700013597900_cit1","doi-asserted-by":"publisher","first-page":"356","DOI":"10.1093\/nsr\/nwx123","article-title":"Design strategies of\nhighly selective nickel catalysts for H2 production via\nhydrous hydrazine decomposition: a review","volume":"5","author":"He","year":"2018","journal-title":"Natl.\nSci. 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Eng.\nJ."},{"issue":"10","key":"2026102700013597900_cit31","first-page":"957","article-title":"Fluorescence Quantum Yield and Ionization\nConstant of Umbelliferone","volume":"74","author":"Jun","year":"2011","journal-title":"Chemistry"},{"issue":"6","key":"2026102700013597900_cit32","doi-asserted-by":"publisher","first-page":"1816","DOI":"10.1021\/ja038838k","article-title":"Theoretical Study of the Spin Trapping\nof Hydroxyl Radical by Cyclic Nitrones: A Density Functional Theory\nApproach","volume":"126","author":"Villamena","year":"2004","journal-title":"J. Am. Chem. 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