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In this work, we report a rapid synthesis method for polycrystalline transition-metal tetraborides using reactive spark plasma sintering (R-SPS). This method was demonstrated on the synthesis of single-phase manganese tetraboride (MnB4) in a short time, 30 minutes. Starting powders with variable B/Mn molar ratios (4.1, 4.5, 5.0, and 8.0) were subjected to 12 h of high-energy ball milling (HEBM), followed by synthesis and consolidation in a single step using R-SPS in a dynamic vacuum atmosphere. Phase purity was confirmed by powder X-ray diffraction (PXRD); single-phase MnB4 was obtained for B/Mn molar ratio of 4.5 and higher in the temperature range of 850 – 1080°C, while the lower B/Mn molar ratio (4.1) resulted in a mixed-phase (Mn3B4 + MnB4) sample. The crystal structure and lattice parameters estimated from PXRD agree well to those reported for single-crystal MnB4. Thermogravimetric differential thermal analysis (TG/DTA) revealed that MnB4 is stable in air up to 400°C.

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• Creative Commons BY-NC-ND Attribution-NonCommercial-NoDerivs 4.0 International
  

Keyword: borides

Date published: 2025-03-11

Publisher: Elsevier BV

Journal:

• Open Ceramics (ISSN: 26665395) vol. 22 100764

Funding:

• Japan Society for the Promotion of Science
• Japan Science and Technology Agency
• JST-Mirai Program JPMJMI19A1

Manuscript type: Publisher's version (Version of record)

MDR DOI:

First published URL: https://doi.org/10.1016/j.oceram.2025.100764

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Updated at: 2025-11-10 12:30:32 +0900

Published on MDR: 2025-11-10 12:24:29 +0900