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High-Pressure, High-Temperature Syntheses of Super-Hard α-Rhombohedral Boron-rich Solids in the B-C-N-O

Published online by Cambridge University Press:  10 February 2011

Hervé Hubert ,
Laurence A.J. Garvie ,
Bertrand Devouard  and
Paul F. McMillan
Hervé Hubert
Affiliation:
Department of Chemistry & Biochemistry and Arizona State University, Tempe, AZ 85287.
Laurence A.J. Garvie
Affiliation:
Department of Geology, Arizona State University, Tempe, AZ 85287.
Bertrand Devouard
Affiliation:
Department of Geology, Arizona State University, Tempe, AZ 85287.
Paul F. McMillan
Affiliation:
Department of Chemistry & Biochemistry and Arizona State University, Tempe, AZ 85287.
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Abstract

We prepared α-rhombohedral (α-rh.) B-rich materials in the B-C-N-O system at high-pressures and temperatures. Samples were synthesized using a multianvil device and characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and parallel electron energy-loss spectroscopy (PEELS). The B-C-O compounds were obtained by reducing B2O3 with B, or mixtures of B and C between 1 to 10 GPa and 1200° and 1800° C In the B-O system we synthesized boron suboxide (nominally B6O) of high purity, crystallinity, and close to stoichiometric. Quantitative analyses give B6O0.95 and B6O0.77 for high-pressure and room-pressure samples, respectively. Between 4 to 5.5 GPa, B6O formed as macroscopic near-perfect regular icosahedra (to 30 μm in diameter). In the B-C-O system, intermediate phases were prepared showing evidence of solid solution between B4C and B6O. Boron carbide crystals, to 20 μm, containing a significant amount of O, typically B6C1.1O0.33 and B6C1.28O0.31, were grown for mixtures in which B and C were reacted with excess B2O3 at 7.5 GPa and 1700 °C. We also report the first conclusive bulk synthesis of a new boron nitride, B6N1-x. This subnitride was synthesized from B and hexagonal BN at 7.5 GPa and 1700 °C. XRD and PEELS shows that the boron subnitride has the α-rh. B structure and average composition B6N0.92

Type
Research Article
Information
MRS Online Proceedings Library (OPL) , Volume 499: Symposium DD – High Pressure Materials Research , 1997 , 315
Copyright
Copyright © Materials Research Society 1998

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References

REFERENCES

(1) Bundy, F. P.; Hall, H. T.; Strong, H. M.; Wentorf, R. H., Nature 1955, 176, 51.Google Scholar
(2) Wentorf, R. H., J. Chenu Phys. 1957, 26, 956.Google Scholar
(3) Ellison Hayashi, C.; Emond, G. T.; Kuo, S. Y., Abrasion of surfaces with boron suboxide, US patent No 920357,. 1994: U.S.A.Google Scholar
(4) Badzian, A. R., Appl. Phys. Lett. 1988, 53, 2495.Google Scholar
(5) Rizzo, H. F.; Simmons, W. C.; Bielstein, H. O., J. Electrochem. Soc. 1962, 109, 1079.Google Scholar
(6) Lundström, T.; Andreev, Y. G., Mat. Sci. Eng. 1996, A209, 16.Google Scholar
(7) Naslain, R. In: Boron and Refractory Borides; Matkovitch, V. L. Ed.; Springer-Verlag: Berlin, Heidelberg, 1977; 139.Google Scholar
(8) Matkovitch, V. I.; Economy, J. In: Boron and Refractory Borides; Matkovitch, V. I., Ed.; Springer-Verlag: Berlin, Heidelberg, 1977; 78.Google Scholar
(9) Hubert, H.; Devouard, B.; Garvie, L. A. J.; O'Keeffe, M.; Buseck, P. R.; Petuskey, W. T.; McMillan, P. F., Nature in press.Google Scholar
(10) Hubert, H.; Garvie, L. A. J.; Devouard, B.; Buseck, P. R.; Petuskey, W. T.; McMillan, P. F., Chemistry of Materials in press.Google Scholar
(11) Hubert, H.; Garvie, L. A. J.; Buseck, P. R.; Petuskey, W. T.; McMillan, P. F., J. Solid State Chem. in press.Google Scholar
(12) Garvie, L. A. J.; Hubert, H.; Buseck, P. R.; Petuskey, W. T.; McMillan, P. F., J. Solid State Chem. in press.Google Scholar
(13) Saitoh, H.; Yoshida, K.; Yarbrough, W. A., J. Mater. Res. 1993, 8, 8.Google Scholar
(14) Condon, J. B.; Holcombe, C. E.; Johnson, D. H.; Steckel, L. M., Inorg. Chem. 1976, 15, 2173.Google Scholar
(15) Walker, D.; Carpenter, M. A.; Hitch, C. M., American Mineralogist 1990, 75, 1020.Google Scholar
(16) Higashi, L.; Kobayashi, M.; Bernhard, J.; Brodhag, C.; Thévenot, F. In: Boron-Rich Solids, A.I.P. Conference and Proceedings; Emin, D.; Aselage, T.; Beckel, C. L.; Howard, I. A.; Wood, C. Ed.; 1991; 231, 201.Google Scholar
(17) Petrak, D. R.; Ruh, R.; Goosey, B. F. In: 5th Materials Research Symposium; ed.; NBS Spec. Pub.: 1972; 364, 605.Google Scholar
(18) Bolmgren, H.; Lundström, T.; Okada, S. In: Boron-Rich Solids, A.I.P. Conference and Proceedings; Emin, D.; Aselage, T.; Beckel, C. L.; Howard, I. A.; Wood, C. Ed.; 1991; 231, 197.Google Scholar
(19) Brodhag, C.; Thévenot, F., J. Less-Common Met. 1986, 117, 1.Google Scholar
(20) LaPlaca, S.; Post, B., Planseeber. Pulvermet. 1961, 9, 109.Google Scholar
(21) Lundström, T.; Bolmgren, H. In: 11th International Symposium on Boron, Borides and Related Compounds; Uno, R.; Higashi, L. Ed.; JJAP Series: Tsukuba, 1994; 10, 1.Google Scholar
(22) Pasternak, R. A., Acta Crystallogr. 1959, 12, 612.Google Scholar
(23) Liu, X.; Zhao, X.; Hou, W.; Su, W., J. Alloys Comp. 1995, 223, L5.Google Scholar
(24) Larson, A. C. In: Boron-rich solids, AIP Conference Proceedings; Emin, D.; Aselage, T.; Beckel, C. L.; Howard, I. A.; Wood, C. Ed.; American Institute of Physics: New-York, 1986; 140, 109.Google Scholar