Lamellar α-MoO₃ nanostructured powders from additive-free aqueous precipitation and brief milling: band-gap tuning without phase transformation

Lamellar α-MoO₃ nanostructured powders from additive-free aqueous precipitation and brief milling: band-gap tuning without phase transformation | 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 Lamellar α-MoO₃ nanostructured powders from additive-free aqueous precipitation and brief milling: band-gap tuning without phase transformation Loundja Chibane, Rosa María Aranda, Saifi Amirouche, Jesús Rodríguez Vázquez This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-8042024/v1 This work is licensed under a CC BY 4.0 License Status: Published Journal Publication published 28 Feb, 2026 Read the published version in Journal of Materials Science: Materials in Electronics → Version 1 posted You are reading this latest preprint version Abstract Nanostructured metal oxides are key to next-generation optoelectronic and energy devices, yet performance hinges on synthesis-controlled particle size, phase purity, and defect chemistry. Here, we report an additive-free aqueous precipitation route using ammonium heptamolybdate tetrahydrate (AHM, \(\:(\text{N}{\text{H}}_{4}{)}_{6}\text{M}{\text{o}}_{7}{\text{O}}_{24}\cdot\:4{\text{H}}_{2}\text{O}\) ) at controlled concentrations, followed by annealing at 500°C and brief ball milling (60–120 min), to produce phase-pure, nanostructured α-MoO₃ powders. X-ray diffraction confirms single-phase orthorhombic α-MoO₃; Williamson-Hall analysis indicates milling-time-driven crystallite-size reductions from 52.56 to 15.17 nm in the most dilute series and from 19.73 to 15.26 nm in the more concentrated series. Electron microscopy reveals the formation of α-MoO₃ nanoparticles (~ 20–100 nm) as agglomerates after only 1 h of milling, together with a concomitant transformation from micrometer-long rod-like crystallites to rounded nanoparticles. Energy-dispersive X-ray spectroscopy detects only Mo and O, and high-resolution transmission electron microscopy confirms retention of the characteristic lamellar α-MoO₃ architecture despite milling-induced rounding. Fourier-transform infrared spectroscopy reveals the Mo = O stretching vibration, consistent with the layered orthorhombic phase. UV-Vis diffuse reflectance shows a milling-time-dependent decrease in the optical band gap from 3.72 to 3.66 eV, 3.73 to 3.62 eV, and 3.72 to 3.69 eV for the first, second, and third concentration series, respectively. Overall, with appropriate parameterization, brief mechanical milling lowers the band gap without any phase change or loss of the lamellar architecture, providing a robust, scalable route to tailor α-MoO₃ for various applications in optoelectronics. Corresponding author : Loundja Chibane, Laboratory of Design and Control of Production Systems (L2CSP), Department of Electronics, Faculty of Electrical and Computer Engineering, Mouloud Mammeri University (UMMTO), Algeria. E-mail : [email protected] Nanostructured metal oxides additive-free aqueous precipitation annealing ball milling nanostructured α-MoO₃ powders optoelectronic applications Full Text Additional Declarations No competing interests reported. Cite Share Download PDF Status: Published Journal Publication published 28 Feb, 2026 Read the published version in Journal of Materials Science: Materials in Electronics → Version 1 posted 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. We do this by developing innovative software and high quality services for the global research community. Our growing team is made up of researchers and industry professionals working together to solve the most critical problems facing scientific publishing. Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-8042024","acceptedTermsAndConditions":true,"allowDirectSubmit":true,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":554745865,"identity":"492a7e45-d1b4-4c1e-8764-5af69a5ed0cf","order_by":0,"name":"Loundja Chibane","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAA80lEQVRIiWNgGAWjYBACPhDBwwMkJBjbQGw5qAQzTi1s6FqMgZixgbAWECEBYSc2ENTC3mP24I2MHQP/7Oa2Bz932KRvuHY6/cEHBmt7nFp4zpgbzuFJZpC4c7DdsPdMWu6G27kbG2cwpOO0hk0ix0yah4eZwUAisU2Ct+0wWEszD8NhNgJa6sFaJP+2/U83gGrhIaDlMFiLNG/bgQSYFgncfjlWJjmH5ziPxI3EdmPZtmTDmUAtM2cYpBvg0sLP3rxN4m1PtRz/jPRnD9+22cnz3c7d8OFDBe4QAwPGHgZ0l+O0AwZ+EFIwCkbBKBgFIxoAAIDQTrojdLobAAAAAElFTkSuQmCC","orcid":"","institution":"Mouloud Mammeri University of Tizi-Ouzou (UMMTO)","correspondingAuthor":true,"prefix":"","firstName":"Loundja","middleName":"","lastName":"Chibane","suffix":""},{"id":554745866,"identity":"45c57871-77e5-4527-9c1c-8c9d2e795eac","order_by":1,"name":"Rosa María Aranda","email":"","orcid":"","institution":"University of Huelva","correspondingAuthor":false,"prefix":"","firstName":"Rosa","middleName":"María","lastName":"Aranda","suffix":""},{"id":554745867,"identity":"e8e81a36-b485-45dd-8001-94deffbe60a3","order_by":2,"name":"Saifi Amirouche","email":"","orcid":"","institution":"Scientific and Technical Research Center in Physico-Chemical Analyses (CRAPC)","correspondingAuthor":false,"prefix":"","firstName":"Saifi","middleName":"","lastName":"Amirouche","suffix":""},{"id":554745869,"identity":"682a8d15-2bba-4e3b-a3e2-d15b5b5f4119","order_by":3,"name":"Jesús Rodríguez Vázquez","email":"","orcid":"","institution":"University of Huelva","correspondingAuthor":false,"prefix":"","firstName":"Jesús","middleName":"Rodríguez","lastName":"Vázquez","suffix":""}],"badges":[],"createdAt":"2025-11-05 22:38:12","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-8042024/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-8042024/v1","draftVersion":[],"editorialEvents":[{"content":"https://doi.org/10.1007/s10854-026-16859-z","type":"published","date":"2026-02-28T15:58:52+00:00"}],"editorialNote":"","failedWorkflow":false,"files":[{"id":97668930,"identity":"7cccb30c-a169-4eab-ab49-d8319b6f6840","added_by":"auto","created_at":"2025-12-08 09:26:43","extension":"docx","order_by":0,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":42031245,"visible":true,"origin":"","legend":"","description":"","filename":"Articleforreview1.docx","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/a95437c6d06a2eae712f6db5.docx"},{"id":97668924,"identity":"e16c52e4-5a50-4caf-9d90-7abfbffc526c","added_by":"auto","created_at":"2025-12-08 09:26:41","extension":"json","order_by":1,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":6319,"visible":true,"origin":"","legend":"","description":"","filename":"3a2825d00b1b460fa18c5f7910a4780b.json","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/cea0236a224429a4f8936389.json"},{"id":97469931,"identity":"16ce5b77-68db-451b-ac7c-72e08559755c","added_by":"auto","created_at":"2025-12-04 17:26:15","extension":"xml","order_by":2,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":124402,"visible":true,"origin":"","legend":"","description":"","filename":"3a2825d00b1b460fa18c5f7910a4780b1enriched.xml","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/8a8f875fcd9033f5a58f8f70.xml"},{"id":97668830,"identity":"33ff6caa-cf3a-4e81-837b-1145206eea4b","added_by":"auto","created_at":"2025-12-08 09:26:21","extension":"jpeg","order_by":4,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":62335,"visible":true,"origin":"","legend":"","description":"","filename":"floatimage1.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/f4b11780003e9aac172f68cf.jpeg"},{"id":97469926,"identity":"25f4e8be-8752-4f79-bab2-970cf5c3d477","added_by":"auto","created_at":"2025-12-04 17:26:15","extension":"jpeg","order_by":5,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":15070,"visible":true,"origin":"","legend":"","description":"","filename":"floatimage10.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/409b8f8d98bd696cd0f64e2a.jpeg"},{"id":97668563,"identity":"aa6b6830-7808-4d28-8093-d216139cee30","added_by":"auto","created_at":"2025-12-08 09:25:47","extension":"emf","order_by":6,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":189452,"visible":true,"origin":"","legend":"","description":"","filename":"floatimage11.emf","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/fb486b52bc39444bfb2ec72f.emf"},{"id":97668491,"identity":"180b2a5d-ff06-44ae-adc8-4a9d8552090b","added_by":"auto","created_at":"2025-12-08 09:25:38","extension":"jpeg","order_by":7,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":6782,"visible":true,"origin":"","legend":"","description":"","filename":"floatimage12.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/a14a6c6659322691234daf10.jpeg"},{"id":97668646,"identity":"de21f031-c997-4ad9-9afa-69957ae9b077","added_by":"auto","created_at":"2025-12-08 09:25:56","extension":"jpeg","order_by":8,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":6306,"visible":true,"origin":"","legend":"","description":"","filename":"floatimage13.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/51a38e404b5d407e97872851.jpeg"},{"id":97469932,"identity":"7c7c90c9-5649-490e-9026-7f7046079e51","added_by":"auto","created_at":"2025-12-04 17:26:15","extension":"jpeg","order_by":9,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":433216,"visible":true,"origin":"","legend":"","description":"","filename":"floatimage2.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/3ff2d3f14ec30d00e10a9223.jpeg"},{"id":97469939,"identity":"b4779b30-ba65-465c-aec2-1769c54e9afd","added_by":"auto","created_at":"2025-12-04 17:26:15","extension":"jpeg","order_by":10,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":271684,"visible":true,"origin":"","legend":"","description":"","filename":"floatimage3.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/d00f75f31c4bc0a27eb8ff03.jpeg"},{"id":97669780,"identity":"d76e4909-4669-4e20-86df-d32b58926c9b","added_by":"auto","created_at":"2025-12-08 09:28:52","extension":"jpeg","order_by":11,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":6070,"visible":true,"origin":"","legend":"","description":"","filename":"floatimage4.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/bba205f5f11d80414d5de733.jpeg"},{"id":97668649,"identity":"1227587a-eedf-417e-81b6-53bcdaee3212","added_by":"auto","created_at":"2025-12-08 09:25:56","extension":"jpeg","order_by":12,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":130204,"visible":true,"origin":"","legend":"","description":"","filename":"floatimage5.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/02ccbc87108a216f3324a8c1.jpeg"},{"id":97469928,"identity":"e2a08734-c4cd-4b94-869b-ea255d7b3067","added_by":"auto","created_at":"2025-12-04 17:26:15","extension":"jpeg","order_by":13,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":1074,"visible":true,"origin":"","legend":"","description":"","filename":"floatimage6.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/820ed2513b7d841a17549277.jpeg"},{"id":97668465,"identity":"667e64e7-dc6d-468c-bc2e-161e9e65611e","added_by":"auto","created_at":"2025-12-08 09:25:36","extension":"jpeg","order_by":14,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":7310,"visible":true,"origin":"","legend":"","description":"","filename":"floatimage7.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/12a3fa2de61a074051f5c358.jpeg"},{"id":97668470,"identity":"bd8b5a29-cb2e-4dc4-8416-145ccc7c2c24","added_by":"auto","created_at":"2025-12-08 09:25:36","extension":"jpeg","order_by":15,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":4893,"visible":true,"origin":"","legend":"","description":"","filename":"floatimage8.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/bf9c6c8670ad0e37d9626356.jpeg"},{"id":97669779,"identity":"1a05c49a-ba1e-4df3-8781-34227badb3fc","added_by":"auto","created_at":"2025-12-08 09:28:52","extension":"jpeg","order_by":16,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":12686,"visible":true,"origin":"","legend":"","description":"","filename":"floatimage9.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/c83da5785c45ef637e92d2dc.jpeg"},{"id":97668422,"identity":"cf577371-2ffd-4378-89fc-704cd70ab9f6","added_by":"auto","created_at":"2025-12-08 09:25:32","extension":"jpeg","order_by":17,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":116547,"visible":true,"origin":"","legend":"","description":"","filename":"groupimage1.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/502a9d3a9f27467974cff962.jpeg"},{"id":97669804,"identity":"3dfda86a-e6c2-4363-8ace-97613e764c64","added_by":"auto","created_at":"2025-12-08 09:28:59","extension":"jpeg","order_by":18,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":4484,"visible":true,"origin":"","legend":"","description":"","filename":"groupimage2.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/45c2d56ed2f4d078bca6f00c.jpeg"},{"id":97469943,"identity":"995c8dcf-ca2f-4ef6-9f6f-97351ed33988","added_by":"auto","created_at":"2025-12-04 17:26:15","extension":"jpeg","order_by":19,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":73719,"visible":true,"origin":"","legend":"","description":"","filename":"groupimage3.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/56ac2bdc717ee60f5508d5c2.jpeg"},{"id":97469952,"identity":"f0fe9ab7-9fda-4370-a3cd-49760bfd0d17","added_by":"auto","created_at":"2025-12-04 17:26:15","extension":"jpeg","order_by":20,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":99532,"visible":true,"origin":"","legend":"","description":"","filename":"groupimage4.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/24052e7b41543aa0379c7346.jpeg"},{"id":97669126,"identity":"1f4805e7-40ce-43d7-986a-4e2b3b429795","added_by":"auto","created_at":"2025-12-08 09:27:18","extension":"jpeg","order_by":21,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":42119,"visible":true,"origin":"","legend":"","description":"","filename":"groupimage5.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/e3e9806827df8789cdd45861.jpeg"},{"id":97669517,"identity":"adf01dc7-ddaa-4dc6-a402-256f9c2ab2eb","added_by":"auto","created_at":"2025-12-08 09:28:07","extension":"jpeg","order_by":22,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":43819,"visible":true,"origin":"","legend":"","description":"","filename":"groupimage6.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/440c54968427af827f1fee64.jpeg"},{"id":97669382,"identity":"165befdc-5d85-4c60-9273-8ddf7d4deb0d","added_by":"auto","created_at":"2025-12-08 09:27:54","extension":"png","order_by":23,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":12639,"visible":true,"origin":"","legend":"","description":"","filename":"Onlinefloatimage1.png","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/a2c905774fdacdeeabeeaa44.png"},{"id":97669091,"identity":"0bb0b1cc-1b60-4199-a4f4-4e35d170042b","added_by":"auto","created_at":"2025-12-08 09:27:11","extension":"png","order_by":24,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":1809,"visible":true,"origin":"","legend":"","description":"","filename":"Onlinefloatimage10.png","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/d0df4532b9781f0b66191c3c.png"},{"id":97670342,"identity":"6a1a9575-6bfc-4824-aafd-2b34728b2a4f","added_by":"auto","created_at":"2025-12-08 09:30:21","extension":"png","order_by":25,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":22181,"visible":true,"origin":"","legend":"","description":"","filename":"Onlinefloatimage11.png","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/8741472fd621660d12ebc84b.png"},{"id":97469965,"identity":"b9a0761e-5185-48ec-9fa6-6bb8fc8c758a","added_by":"auto","created_at":"2025-12-04 17:26:16","extension":"png","order_by":26,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":1295,"visible":true,"origin":"","legend":"","description":"","filename":"Onlinefloatimage12.png","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/2706c7ae8f6d671763c4bcb5.png"},{"id":97469946,"identity":"a3515b5e-b528-495a-8bff-253d506a09be","added_by":"auto","created_at":"2025-12-04 17:26:15","extension":"png","order_by":27,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":1272,"visible":true,"origin":"","legend":"","description":"","filename":"Onlinefloatimage13.png","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/e52c950b4a5088fe6a29346a.png"},{"id":97469947,"identity":"bbdcbf45-9ac1-4fad-b3db-97dea9c1697f","added_by":"auto","created_at":"2025-12-04 17:26:15","extension":"png","order_by":28,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":87251,"visible":true,"origin":"","legend":"","description":"","filename":"Onlinefloatimage2.png","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/ae06250bddbcc1675efbc95b.png"},{"id":97469958,"identity":"467b0a1a-a9cf-4cc1-8c10-d8c3260501a1","added_by":"auto","created_at":"2025-12-04 17:26:16","extension":"png","order_by":29,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":73059,"visible":true,"origin":"","legend":"","description":"","filename":"Onlinefloatimage3.png","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/351c4b2fc016655258b25931.png"},{"id":97669029,"identity":"3f6fdcf5-36e5-4807-97eb-0500c4236c06","added_by":"auto","created_at":"2025-12-08 09:27:08","extension":"png","order_by":30,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":1245,"visible":true,"origin":"","legend":"","description":"","filename":"Onlinefloatimage4.png","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/a8ec4437b31b8e7ef1ff0248.png"},{"id":97668305,"identity":"a8ad98ac-4b72-4937-b179-5b3af6caef52","added_by":"auto","created_at":"2025-12-08 09:25:17","extension":"png","order_by":31,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":26336,"visible":true,"origin":"","legend":"","description":"","filename":"Onlinefloatimage5.png","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/68bb3c73121318438fa46d8f.png"},{"id":97469962,"identity":"48a6d454-4a94-4ff6-b3f2-7ae0ebf9da21","added_by":"auto","created_at":"2025-12-04 17:26:16","extension":"png","order_by":32,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":935,"visible":true,"origin":"","legend":"","description":"","filename":"Onlinefloatimage6.png","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/6e79918666752334d3038a8f.png"},{"id":97469956,"identity":"c233eb75-bfb4-4140-8505-819309b967bb","added_by":"auto","created_at":"2025-12-04 17:26:16","extension":"png","order_by":33,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":1305,"visible":true,"origin":"","legend":"","description":"","filename":"Onlinefloatimage7.png","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/032a08c4b0d086446b2b74e0.png"},{"id":97469953,"identity":"f649f20f-6747-40e9-90da-6570c496ef1f","added_by":"auto","created_at":"2025-12-04 17:26:16","extension":"png","order_by":34,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":1617,"visible":true,"origin":"","legend":"","description":"","filename":"Onlinefloatimage8.png","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/d788b0b4f03462c45189949b.png"},{"id":97469964,"identity":"26ddc6b2-b183-4e26-82a1-75948f4fc650","added_by":"auto","created_at":"2025-12-04 17:26:16","extension":"png","order_by":35,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":2999,"visible":true,"origin":"","legend":"","description":"","filename":"Onlinefloatimage9.png","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/1c47bfc727def25bf4979168.png"},{"id":97469955,"identity":"6b9302b4-75f1-4909-8151-a82d3796b5b5","added_by":"auto","created_at":"2025-12-04 17:26:16","extension":"png","order_by":36,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":215916,"visible":true,"origin":"","legend":"","description":"","filename":"Onlinegroupimage1.png","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/2c43adb5d8a5b8bae81933a6.png"},{"id":97469960,"identity":"58ec9f41-6f65-4fd7-85b2-4f372473f254","added_by":"auto","created_at":"2025-12-04 17:26:16","extension":"png","order_by":37,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":1090,"visible":true,"origin":"","legend":"","description":"","filename":"Onlinegroupimage2.png","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/398d389b626565b6f5894ea9.png"},{"id":97469950,"identity":"958fb67c-b9ac-445c-9803-1e450b91ce4a","added_by":"auto","created_at":"2025-12-04 17:26:15","extension":"png","order_by":38,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":24991,"visible":true,"origin":"","legend":"","description":"","filename":"Onlinegroupimage3.png","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/a463ed7963a2952c4a223ac7.png"},{"id":97469957,"identity":"d5363898-0b49-456c-9842-52c770192f55","added_by":"auto","created_at":"2025-12-04 17:26:16","extension":"png","order_by":39,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":38431,"visible":true,"origin":"","legend":"","description":"","filename":"Onlinegroupimage4.png","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/ea2f403359195dfcfc0f5676.png"},{"id":97469961,"identity":"e6f463bb-1780-4cf9-89e0-007f11bcd7c0","added_by":"auto","created_at":"2025-12-04 17:26:16","extension":"png","order_by":40,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":9248,"visible":true,"origin":"","legend":"","description":"","filename":"Onlinegroupimage5.png","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/7b2c556103062af5adfee793.png"},{"id":97469967,"identity":"fdad117c-0124-4850-b44b-d26e3bb7f7a3","added_by":"auto","created_at":"2025-12-04 17:26:16","extension":"png","order_by":41,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":14506,"visible":true,"origin":"","legend":"","description":"","filename":"Onlinegroupimage6.png","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/cf6b3c3cc3ef1b86408b170d.png"},{"id":97469963,"identity":"815c844b-6dcc-4bf4-8d8b-bd27f4b38ce4","added_by":"auto","created_at":"2025-12-04 17:26:16","extension":"xml","order_by":42,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":120555,"visible":true,"origin":"","legend":"","description":"","filename":"3a2825d00b1b460fa18c5f7910a4780b1structuring.xml","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/dd271bb165d50b3b32610b47.xml"},{"id":97669387,"identity":"895cd785-aee4-4016-aba7-4e8028eb6247","added_by":"auto","created_at":"2025-12-08 09:27:55","extension":"html","order_by":43,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":134795,"visible":true,"origin":"","legend":"","description":"","filename":"earlyproof.html","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1/d1605d9c570e9ae426e69b13.html"},{"id":103766496,"identity":"be654844-0160-459e-9f00-e5ca0826ce07","added_by":"auto","created_at":"2026-03-02 16:14:47","extension":"pdf","order_by":1,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":1249856,"visible":true,"origin":"","legend":"","description":"","filename":"Articleforreview1.pdf","url":"https://assets-eu.researchsquare.com/files/rs-8042024/v1_covered_5e9b843a-c80d-4696-9cc2-b5122d843672.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"Lamellar α-MoO₃ nanostructured powders from additive-free aqueous precipitation and brief milling: band-gap tuning without phase transformation","fulltext":[],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":false,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":true,"highlight":"","institution":"","isAcceptedByJournal":true,"isAuthorSuppliedPdf":true,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":true,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true},"keywords":"Nanostructured metal oxides, additive-free aqueous precipitation, annealing, ball milling, nanostructured α-MoO₃ powders, optoelectronic applications","lastPublishedDoi":"10.21203/rs.3.rs-8042024/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-8042024/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eNanostructured metal oxides are key to next-generation optoelectronic and energy devices, yet performance hinges on synthesis-controlled particle size, phase purity, and defect chemistry. Here, we report an additive-free aqueous precipitation route using ammonium heptamolybdate tetrahydrate (AHM, \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\:(\\text{N}{\\text{H}}_{4}{)}_{6}\\text{M}{\\text{o}}_{7}{\\text{O}}_{24}\\cdot\\:4{\\text{H}}_{2}\\text{O}\\)\u003c/span\u003e\u003c/span\u003e) at controlled concentrations, followed by annealing at 500\u0026deg;C and brief ball milling (60\u0026ndash;120 min), to produce phase-pure, nanostructured α-MoO₃ powders. X-ray diffraction confirms single-phase orthorhombic α-MoO₃; Williamson-Hall analysis indicates milling-time-driven crystallite-size reductions from 52.56 to 15.17 nm in the most dilute series and from 19.73 to 15.26 nm in the more concentrated series. Electron microscopy reveals the formation of α-MoO₃ nanoparticles (~\u0026thinsp;20\u0026ndash;100 nm) as agglomerates after only 1 h of milling, together with a concomitant transformation from micrometer-long rod-like crystallites to rounded nanoparticles. Energy-dispersive X-ray spectroscopy detects only Mo and O, and high-resolution transmission electron microscopy confirms retention of the characteristic lamellar α-MoO₃ architecture despite milling-induced rounding. Fourier-transform infrared spectroscopy reveals the Mo\u0026thinsp;=\u0026thinsp;O stretching vibration, consistent with the layered orthorhombic phase. UV-Vis diffuse reflectance shows a milling-time-dependent decrease in the optical band gap from 3.72 to 3.66 eV, 3.73 to 3.62 eV, and 3.72 to 3.69 eV for the first, second, and third concentration series, respectively. Overall, with appropriate parameterization, brief mechanical milling lowers the band gap without any phase change or loss of the lamellar architecture, providing a robust, scalable route to tailor α-MoO₃ for various applications in optoelectronics.\u003c/p\u003e\u003cp\u003e\u003cb\u003eCorresponding author\u003c/b\u003e: Loundja Chibane, Laboratory of Design and Control of Production Systems (L2CSP), Department of Electronics, Faculty of Electrical and Computer Engineering, Mouloud Mammeri University (UMMTO), Algeria.\u003c/p\u003e\u003cp\u003e\u003cb\u003eE-mail\u003c/b\u003e: [email protected]\u003c/p\u003e","manuscriptTitle":"Lamellar α-MoO₃ nanostructured powders from additive-free aqueous precipitation and brief milling: band-gap tuning without phase transformation","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2025-12-04 17:26:10","doi":"10.21203/rs.3.rs-8042024/v1","editorialEvents":[{"type":"communityComments","content":0}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true}}],"origin":"","ownerIdentity":"635368ed-5875-4a96-a65d-e088ff0fa5dc","owner":[],"postedDate":"December 4th, 2025","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"posted","subjectAreas":[],"tags":[],"updatedAt":"2026-03-02T16:12:47+00:00","versionOfRecord":{"articleIdentity":"rs-8042024","link":"https://doi.org/10.1007/s10854-026-16859-z","journal":{"identity":"journal-of-materials-science-materials-in-electronics","isVorOnly":false,"title":"Journal of Materials Science: Materials in Electronics"},"publishedOn":"2026-02-28 15:58:52","publishedOnDateReadable":"February 28th, 2026"},"versionCreatedAt":"2025-12-04 17:26:10","video":"","vorDoi":"10.1007/s10854-026-16859-z","vorDoiUrl":"https://doi.org/10.1007/s10854-026-16859-z","workflowStages":[]},"version":"v1","identity":"rs-8042024","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-8042024","identity":"rs-8042024","version":["v1"]},"buildId":"8U1c8b4HqxoKbykW_rLl7","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}