Synergistic Engineering of Nanoporous Structure and Surface Chemistry via Ultrasound-Assisted Oxidative Reactivation for Enhanced NO Adsorption

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Abstract A “ultrasound-assisted oxidative reactivation” strategy was developed to precisely tune nanoscale porosity and interfacial chemistry of viscose-based activated carbon fibers (VACFs). Upon moderate H 2 O 2 oxidation, micropores in the 0.5-1.0 nm range were significantly enriched, accompanied by the generation of limited mesopores. Concurrently, surface functionalities evolved from C–O toward C = O and –OH groups, enhancing wall polarity and enabling synergistic physisorption–chemisorption of NO. Structure-activity relationship analysis revealed that efficient capture occurs when the kinetic diameter of NO (0.317 nm) matches pore sizes within the confinement window of 0.54–0.95 nm, whereas excessive alkaline activation collapsed micropores and deteriorated adsorption. Oxygenated groups further facilitated dipole and hydrogen-bond interactions, and under oxygen-containing atmospheres, catalyzed NO oxidation to NO 2 with subsequent capture, amplifying removal capacity. The optimized condition (10 wt% H 2 O 2 , 80°C, 5 h) maximized micropore fraction and tailored surface chemistry without compromising the microcrystalline framework, resulting in superior NO adsorption. This work demonstrates an effective route for structural and interfacial engineering of VACFs, offering a broadly applicable basis for dual matching in molecular size and polarity toward multi-pollutant control.
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Synergistic Engineering of Nanoporous Structure and Surface Chemistry via Ultrasound-Assisted Oxidative Reactivation for Enhanced NO Adsorption | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Research Article Synergistic Engineering of Nanoporous Structure and Surface Chemistry via Ultrasound-Assisted Oxidative Reactivation for Enhanced NO Adsorption Liyuan Yu, Xiangkun Nie, Kai Zhang, Chong Chi, Junwei Yu, Bo Zhu This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-7940238/v1 This work is licensed under a CC BY 4.0 License Status: Under Review Version 1 posted 11 You are reading this latest preprint version Abstract A “ultrasound-assisted oxidative reactivation” strategy was developed to precisely tune nanoscale porosity and interfacial chemistry of viscose-based activated carbon fibers (VACFs). Upon moderate H 2 O 2 oxidation, micropores in the 0.5-1.0 nm range were significantly enriched, accompanied by the generation of limited mesopores. Concurrently, surface functionalities evolved from C–O toward C = O and –OH groups, enhancing wall polarity and enabling synergistic physisorption–chemisorption of NO. Structure-activity relationship analysis revealed that efficient capture occurs when the kinetic diameter of NO (0.317 nm) matches pore sizes within the confinement window of 0.54–0.95 nm, whereas excessive alkaline activation collapsed micropores and deteriorated adsorption. Oxygenated groups further facilitated dipole and hydrogen-bond interactions, and under oxygen-containing atmospheres, catalyzed NO oxidation to NO 2 with subsequent capture, amplifying removal capacity. The optimized condition (10 wt% H 2 O 2 , 80°C, 5 h) maximized micropore fraction and tailored surface chemistry without compromising the microcrystalline framework, resulting in superior NO adsorption. This work demonstrates an effective route for structural and interfacial engineering of VACFs, offering a broadly applicable basis for dual matching in molecular size and polarity toward multi-pollutant control. Reactivation NO adsorption properties Viscose-based activated carbon fiber Interface microenvironment Full Text Additional Declarations No competing interests reported. Supplementary Files 1.GraphicalAbstract.doc 1.Highlights.docx Cite Share Download PDF Status: Under Review Version 1 posted Editorial decision: Revision requested 16 Mar, 2026 Reviews received at journal 07 Mar, 2026 Reviews received at journal 27 Feb, 2026 Reviewers agreed at journal 16 Feb, 2026 Reviewers agreed at journal 02 Feb, 2026 Reviewers agreed at journal 27 Nov, 2025 Reviewers agreed at journal 21 Nov, 2025 Reviewers invited by journal 21 Nov, 2025 Editor assigned by journal 24 Oct, 2025 Submission checks completed at journal 24 Oct, 2025 First submitted to journal 24 Oct, 2025 You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. As a division of Research Square Company, we’re committed to making research communication faster, fairer, and more useful. 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Upon moderate H\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e2\u003c/sub\u003e oxidation, micropores in the 0.5-1.0 nm range were significantly enriched, accompanied by the generation of limited mesopores. Concurrently, surface functionalities evolved from C\u0026ndash;O toward C\u0026thinsp;=\u0026thinsp;O and \u0026ndash;OH groups, enhancing wall polarity and enabling synergistic physisorption\u0026ndash;chemisorption of NO. Structure-activity relationship analysis revealed that efficient capture occurs when the kinetic diameter of NO (0.317 nm) matches pore sizes within the confinement window of 0.54\u0026ndash;0.95 nm, whereas excessive alkaline activation collapsed micropores and deteriorated adsorption. Oxygenated groups further facilitated dipole and hydrogen-bond interactions, and under oxygen-containing atmospheres, catalyzed NO oxidation to NO\u003csub\u003e2\u003c/sub\u003e with subsequent capture, amplifying removal capacity. The optimized condition (10 wt% H\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e2\u003c/sub\u003e, 80\u0026deg;C, 5 h) maximized micropore fraction and tailored surface chemistry without compromising the microcrystalline framework, resulting in superior NO adsorption. 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