Akbari, AmirSuzer-Cicek, IlaydaMertdinc-Ulkuseven, SiddikaGokce, HasanOvecoglu, M. LutfiAgaogullari, Duygu2026-01-052026-01-0520250972-28150975-1645https://doi.org/10.1007/s12666-025-03739-zhttps://hdl.handle.net/20.500.11779/3167This study reports on the thermochemical calculations, mechanochemical synthesis, purification process, and characterization studies of the HfB2 powders by using native sources. Firstly, HfO2, native B2O3, and Mg starting powders were prepared with a multi-axial vibratory ball mill (NanoMultimix) in stoichiometric and excess amounts. The milling process was optimized by varying the time (2, 4, 6, 8, 10, 12 h). Then, unwanted by-products (HfO2, MgO) were removed by leaching with 4 and 6 M HCl. Phase and Rietveld analysis, microstructure investigations with scanning electron microscopy/energy dispersion spectroscopy and transmission electron microscopy, and particle size measurement were conducted. The purest HfB2 was obtained in the powders milled for 8 h in stoichiometric ratios and leached with 6 M HCl. The resulting optimum powder has an average particle size of 135 nm. Oxidation kinetics (500, 600, 700, 800, and 900 degrees C) were also investigated. As the temperature increased, the amount of oxidation increased based on the TG result. As a result of the characterization studies, the synthesis of single-phase, high-purity HfB2 was achieved using domestic resources.eninfo:eu-repo/semantics/closedAccessHafnium DiborideSolid-State ReactionMechanochemical SynthesisPurificationMicrostructural PropertiesArticle10.1007/s12666-025-03739-z2-s2.0-105023479584