Synthesized NiO Nanostructures via Sol–Gel: Unveiling the Role of Annealing Conditions on Structural and Antioxidant Properties

Synthesized NiO Nanostructures via Sol–Gel: Unveiling the Role of Annealing Conditions on Structural and Antioxidant Properties | 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 Synthesized NiO Nanostructures via Sol–Gel: Unveiling the Role of Annealing Conditions on Structural and Antioxidant Properties Azariun Valinia, Rostam Moradian, Masome NaseriTekyeh This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-7926126/v1 This work is licensed under a CC BY 4.0 License Status: Under Review Version 1 posted 10 You are reading this latest preprint version Abstract NiO octahedral nanoparticles were synthesized via the sol–gel method and subsequently characterized using XRD, SEM, and FTIR techniques. By XRD analysis of our results the influence of annealing temperature and time duration on the structural and morphological nanoparticles investigated. The synthesized NiO nanostructures predominantly crystallized in a face-centered cubic (fcc) phase, except for the sample annealed at 300°C. From the XRD data lattice constant obtained. The analysis revealed that increasing the annealing temperature promoted nanoparticle growth. By extending annealing time duration, first crystallite size reduced, then it remained fixed at longer times. The antioxidant potential of the NiO nanoparticles was further assessed using the DPPH radical scavenging assay. Notably, the sample annealed at 400°C for 24 h exhibited significantly enhanced antioxidant activity (76.12 ± 3.43%) compared with the other conditions, highlighting the crucial role of thermal treatment in tailoring both the structural evolution and functional performance of NiO nanomaterials. NiO Octahedral morphology Sol-gel method Structural properties Antioxidant Properties Full Text Additional Declarations No competing interests reported. Cite Share Download PDF Status: Under Review Version 1 posted Editorial decision: Revision requested 12 Dec, 2025 Reviews received at journal 11 Dec, 2025 Reviewers agreed at journal 03 Dec, 2025 Reviews received at journal 05 Nov, 2025 Reviewers agreed at journal 02 Nov, 2025 Reviewers agreed at journal 31 Oct, 2025 Reviewers invited by journal 31 Oct, 2025 Editor assigned by journal 24 Oct, 2025 Submission checks completed at journal 24 Oct, 2025 First submitted to journal 22 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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By XRD analysis of our results the influence of annealing temperature and time duration on the structural and morphological nanoparticles investigated. The synthesized NiO nanostructures predominantly crystallized in a face-centered cubic (fcc) phase, except for the sample annealed at 300\u0026deg;C. From the XRD data lattice constant obtained. The analysis revealed that increasing the annealing temperature promoted nanoparticle growth. By extending annealing time duration, first crystallite size reduced, then it remained fixed at longer times. The antioxidant potential of the NiO nanoparticles was further assessed using the DPPH radical scavenging assay. 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