Thermal stability of hexagonal OsB2

Autor: Zhilin Xie, David A. Cullen, Nina Orlovskaya, E. Andrew Payzant, Richard G. Blair
Rok vydání: 2014
Předmět:
Zdroj: Journal of Solid State Chemistry. 219:210-219
ISSN: 0022-4596
DOI: 10.1016/j.jssc.2014.07.035
Popis: The synthesis of novel hexagonal ReB{sub 2}-type OsB{sub 2} ceramic powder was performed by high energy ball milling of elemental Os and B powders. Two different sources of B powder have been used for this mechanochemical synthesis. One B powder consisted of a mixture of amorphous and crystalline phases and a mixture of {sup 10}B and {sup 11}B isotopes with a fine particle size, while another B powder was a purely crystalline (rhombohedral) material consisting of enriched {sup 11}B isotope with coarse particle size. The same Os powder was used for the synthesis in both cases. It was established that, in the first case, the hexagonal OsB{sub 2} phase was the main product of synthesis with a small quantity of Os{sub 2}B{sub 3} phase present after synthesis as an intermediate product. In the second case, where coarse crystalline {sup 11}B powder was used as a raw material, only Os{sub 2}B{sub 3} boride was synthesized mechanochemically. The thermal stability of hexagonal OsB{sub 2} powder was studied by heating under argon up to 876 °C and cooling in vacuo down to −225 °C. During the heating, the sacrificial reaction 2OsB{sub 2}+3O{sub 2}→2Os+2B{sub 2}O{sub 3} took place due to presence of O{sub 2}/watermore » vapor molecules in the heating chamber, resulting in the oxidation of B atoms and formation of B{sub 2}O{sub 3} and precipitation of Os metal out of the OsB{sub 2} lattice. As a result of such phase changes during heating, the lattice parameters of hexagonal OsB{sub 2} changed significantly. The shrinkage of the a lattice parameter was recorded in 276–426 °C temperature range upon heating, which was attributed to the removal of B atoms from the OsB{sub 2} lattice due to oxidation followed by the precipitation of Os atoms and formation of Os metal. While significant structural changes occurred upon heating due to presence of O{sub 2}, the hexagonal OsB{sub 2} ceramic demonstrated good phase stability upon cooling in vacuo with linear shrinkage of the lattice parameters and no phase changes detected during cooling. - Graphical abstract: The in situ high temperature XRD contour plot (A) and XRD patterns (B) of h-OsB{sub 2} upon heating and cooling under an argon atmosphere. - Highlights: • Different boron sources were compared for the synthesis of h-OsB{sub 2}. • The phase stability and thermal behavior of h-OsB{sub 2} were studied by in situ XRD. • Shrinkage of the a lattice parameter was observed from 276 °C to 426 °C upon heating. • Oxidation of OsB{sub 2} produced B vacancies led to the shrinkage of a lattice parameter.« less
Databáze: OpenAIRE
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