Novel high pressure hexagonal OsB{sub 2} by mechanochemistry
- Department of Mechanical and Aerospace Engineering, University of Central Florida, Orlando, FL 32816 (United States)
- Center for Nanophase Materials Sciences, Oak Ridge National Laboratory, 1 Bethel Valley Road, Oak Ridge, TN 37831 (United States)
- Materials Science and Technology Division, Oak Ridge National Laboratory, Oak Ridge, TN 37831 (United States)
- Department of Chemistry, University of Central Florida, Orlando, FL 32816 (United States)
Hexagonal OsB{sub 2}, a theoretically predicted high-pressure phase, has been synthesized for the first time by a mechanochemical method, i.e., high energy ball milling. X-ray diffraction indicated that formation of hexagonal OsB{sub 2} begins after 2.5 h of milling, and the reaction reaches equilibrium after 18 h of milling. Rietveld refinement of the powder data indicated that hexagonal OsB{sub 2} crystallizes in the P63/mmc space group (No. 194) with lattice parameters of a=2.916 Å and c=7.376 Å. Transmission electron microscopy confirmed the appearance of the hexagonal OsB{sub 2} phase after high energy ball milling. in situ X-ray diffraction experiments showed that the phase is stable from −225 °C to 1050 °C. The hexagonal OsB{sub 2} powder was annealed at 1050 °C for 6 days in vacuo to improve crystallinity and remove strain induced during the mechanochemical synthesis. The structure partially converted to the orthorhombic phase (20 wt%) after fast current assisted sintering of hexagonal OsB{sub 2} at 1500 °C for 5 min. Mechanochemical approaches to the synthesis of hard boride materials allow new phases to be produced that cannot be prepared using conventional methods. - Graphical abstract: High resolution transmission electron micrograph of hexagonal OsB{sub 2} nanocrystallite with corresponding fast Fourier transform and simulated diffraction pattern. - Highlights: • Hexagonal OsB{sub 2} has been synthesized for the first time by mechanochemical method. • Hexagonal OsB{sub 2} crystallizes in P63/mmc space group (No. 194), a=2.916 Å and c=7.376 Å. • The hexagonal structure was confirmed by a transmission electron microscope. • No phase transformation was observed after being annealed at 1050 °C for 6 days. • 20 wt% of h-OsB{sub 2} was transformed to o-OsB{sub 2} after being sintered at 1500 °C for 5 min.
- OSTI ID:
- 22334255
- Journal Information:
- Journal of Solid State Chemistry, Vol. 215; Other Information: Copyright (c) 2014 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; Country of input: International Atomic Energy Agency (IAEA); ISSN 0022-4596
- Country of Publication:
- United States
- Language:
- English
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