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Polycrystalline nanospheres and highly crystalline nanocubes with an equivalent diameter\/body diagonal of 135 nm were synthesized via solvothermal and thermal decomposition methods, respectively. Scanning electron microscopy (SEM) revealed that the nanospheres developed smoother surfaces and gradually transformed toward a cubic morphology upon annealing, with increasing temperature and duration. Vibrating sample magnetometry (VSM) measurements showed that both saturation magnetization and coercivity increased with annealing as the particles evolved toward cube-like morphology and larger crystallite size, indicating that the magnetic properties of Fe3O4 nanoparticles are strongly dependent on crystallite size and shape. Nanospheres annealed between 500 and 850 \u00b0C exhibited increases in both crystallite size and saturation magnetization; however, coercivity decreased at 850 \u00b0C, where the crystallite size was maximal. Annealing at 700 \u00b0C for 12 h resulted in enhanced crystallite size and improved magnetic properties. Prolonged annealing at 700 \u00b0C (24 h) yielded the largest crystallite size but led to a significant reduction in saturation magnetization. This study demonstrates a clear correlation between magnetic properties, crystallinity, and morphology in nanoparticles beyond the superparamagnetic size regime (e.g., 135 nm). It further provides a strategy for tuning structural parameters that govern magnetic behavior and establishes an alternative, more facile route to obtain Fe3O4 nanospheres with crystallite sizes and magnetic properties comparable to nanocubes obtained via direct synthesis.<\/jats:p>","DOI":"10.3390\/ma19132911","type":"journal-article","created":{"date-parts":[[2026,7,7]],"date-time":"2026-07-07T09:53:46Z","timestamp":1783418026000},"page":"2911","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Tuning the Crystallite Size, Shape, and Magnetic Properties of Fe3O4 Nanoparticles Using Annealing"],"prefix":"10.3390","volume":"19","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-2368-2468","authenticated-orcid":false,"given":"Riddhiman","family":"Medhi","sequence":"first","affiliation":[{"name":"Department of Chemistry, University of Scranton, 800 Linden Street, Scranton, PA 18510, USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-5703-2674","authenticated-orcid":false,"given":"Arati G.","family":"Kolhatkar","sequence":"additional","affiliation":[{"name":"Department of Chemistry and the Texas Center for Superconductivity, University of Houston, Houston, TX 77204, USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yi-Ting","family":"Chen","sequence":"additional","affiliation":[{"name":"Department of Chemistry and the Texas Center for Superconductivity, University of Houston, Houston, TX 77204, USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-4604-8726","authenticated-orcid":false,"given":"Mohammad","family":"Khodadadi","sequence":"additional","affiliation":[{"name":"Department of Electrical and Computer Engineering, University of Houston, Houston, TX 77204, USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-5710-1601","authenticated-orcid":false,"given":"Nhat","family":"Ngo","sequence":"additional","affiliation":[{"name":"Department of Chemistry and the Texas Center for Superconductivity, University of Houston, Houston, TX 77204, USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Rohan","family":"Dhall","sequence":"additional","affiliation":[{"name":"National Center for Electron Microscopy, Molecular Foundry, Lawrence Berkeley National Laboratory, Berkeley, CA 94720, USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jacob","family":"Magdon","sequence":"additional","affiliation":[{"name":"Department of Chemistry, University of Scranton, 800 Linden Street, Scranton, PA 18510, USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Pailinrut","family":"Chinwangso","sequence":"additional","affiliation":[{"name":"Department of Chemistry and the Texas Center for Superconductivity, University of Houston, Houston, TX 77204, USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Alba M.","family":"Valero","sequence":"additional","affiliation":[{"name":"Department of Engineering Technology, University of Houston, Houston, TX 77204, USA"},{"name":"Advanced Manufacturing Institute, University of Houston, Houston, TX 77204, USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-5587-0802","authenticated-orcid":false,"given":"Francisco C.","family":"Robles Hernandez","sequence":"additional","affiliation":[{"name":"Department of Engineering Technology, University of Houston, Houston, TX 77204, USA"},{"name":"Advanced Manufacturing Institute, University of Houston, Houston, TX 77204, USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-2272-562X","authenticated-orcid":false,"given":"Dimitri","family":"Litvinov","sequence":"additional","affiliation":[{"name":"Department of Electrical and Computer Engineering, University of Houston, Houston, TX 77204, USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-9584-8861","authenticated-orcid":false,"given":"T. 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