{"title":"Rapid synthesis of manganese tetraboride (MnB4) using reactive spark plasma sintering","authors":"S.B. Dhuban , Hyoung-Won Son , Takao Mori","doi":"10.1016/j.oceram.2025.100764","DOIUrl":null,"url":null,"abstract":"<div><div>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 manganese tetraboride (MnB<sub>4</sub>) in a short time, 30 min. 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); MnB<sub>4</sub> 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 (Mn<sub>3</sub>B<sub>4</sub> + MnB<sub>4</sub>) sample. The crystal structure and lattice parameters estimated from PXRD agree well to those reported for single-crystal MnB<sub>4</sub>. Thermogravimetric differential thermal analysis (TG/DTA) revealed that MnB<sub>4</sub> is stable in air up to 400 °C.</div></div>","PeriodicalId":34140,"journal":{"name":"Open Ceramics","volume":"22 ","pages":"Article 100764"},"PeriodicalIF":2.8000,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Open Ceramics","FirstCategoryId":"1085","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S2666539525000318","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"2025/3/10 0:00:00","PubModel":"Epub","JCR":"Q1","JCRName":"MATERIALS SCIENCE, CERAMICS","Score":null,"Total":0}
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Abstract
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 manganese tetraboride (MnB4) in a short time, 30 min. 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); 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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