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Formation of zirconium diboride and other metal borides by volume combustion synthesis and mechanochemical process
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Date
2008
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Akgün, Barış
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The aim of this study was to produce zirconium diboride (ZrB2) and other metal borides such as lanthanum hexaboride (LaB6) and cerium hexaboride (CeB6) by magnesiothermic reduction (reaction of metal oxide, boron oxide and magnesium) using volume combustion synthesis (VCS) and mechanochemical process (MCP). Production of ZrB2 by VCS in air occurred with the formation of side products, Zr2ON2 and Mg3B2O6 in addition to MgO. Formation of Zr2ON2 was prevented by conducting VCS experiments under argon atmosphere. Wet ball milling was applied before leaching for easier removal of Mg3B2O6. Leaching in 5 M HCl for 2.5 hours was found to be sufficient for removal of MgO and Mg3B2O6. By MCP, 30 hours of ball milling was enough to produce ZrB2 where 10% of excess Mg and B2O3 were used. MgO was easily removed when MCP products were leached in 1 M HCl for 30 minutes. Complete reduction of ZrO2 could not be achieved in either production method because of the stability of ZrO2. Hence, after leaching VCS or MCP products, final product was composed of ZrB2 and ZrO2. Formation of LaB6 and CeB6 were very similar to each other via both methods. Mg3B2O6 appeared as a side product in the formation of both borides by VCS. After wet ball milling, products were leached in 1 M HCl for 15 hours and pure LaB6 or CeB6 was obtained. As in ZrB2 production, 30 hours of ball milling was sufficient to form these hexaborides by MCP. MgO was removed after leaching in 1 M HCl for 30 minutes and the desired hexaboride was obtained in pure form.
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http://etd.lib.metu.edu.tr/upload/2/12609229/index.pdf
https://hdl.handle.net/11511/17469
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Graduate School of Natural and Applied Sciences, Thesis
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B. Akgün, “Formation of zirconium diboride and other metal borides by volume combustion synthesis and mechanochemical process,” M.S. - Master of Science, Middle East Technical University, 2008.