Abstract
Reactions between titanium and microcrystalline boron powders in a Na2B4O7 ionic melt at temperatures from 700 to 850°C and those between TiCl4 and NaBH4 at temperatures from 300 to 750°C and hydrogen pressures of up to 10 MPa, with no solvent, have been studied by X-ray diffraction, scanning electron microscopy, thermogravimetry, and elemental analysis. The results demonstrate that TiB2 formation occurs at t 〉 730°C and 550°C, respectively. According to scanning electron microscopy data, the TiB2 powder consists of particles 70–75 and 35–50 nm size, and the crystallite size evaluated from X-ray diffraction data is 55 and 30 nm, respectively, in agreement with the equivalent particle diameters obtained from the specific surface area of the TiB2 powders: 60 and 45 nm, respectively.
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Samsonov, G.V. and Vinnitskii, I.M., Tugoplavkie soedineniya. Spravochnik (Refractory Compounds: A Handbook), Moscow: Metallurgiya, 1976.
Andrievskii, R.A., Osnovy nanostrukturnogo materialovedeniya. Vozmozhnosti i problemy (Principles of Nanostructured Materials Research), Moscow: BINOM. Laboratoriya Znanii, 2012.
Kobayashi, N., Vvedenie v nanotekhnologiyu (Introduction to Nanotechnology), Moscow: Binom. Laboratoriya Znanii, 2005 (translated from Japanese).
Gogotsi, Yu., Nanomaterials Handbook, London: Taylor & Francis, 2006.
Jensen, J.A., Gozum, J.E., Pollina, D.M., and Girolami, G.S., Titanium, zirconium and hafnium tetrahydroborates as “tailored” CVD precursors for metal diboride thin films, J. Am. Chem. Soc., 1988, vol. 110, no. 5, pp. 1643–1644.
Rice, G.W. and Woodin, R.L., Zirconium borohydride as a zirconium boride precursors, J. Am. Chem. Soc., 1988, vol. 71, no. 4, pp. 181–183.
Wayda, A.L., Schneemeyer, L.F., and Opila, R.L., A low-temperature film deposition of zirconium and hafnium borides for the borohydrides, M(BH4)4, Appl. Phys. Lett., 1988, vol. 53, no. 5, pp. 361–363.
Andrievski, R.A., Kravchenko, S.E., and Shilkin, S.P., Some properties of ultrafine zirconium boride powders and films, Jpn. J. Appl. Phys., 1994, vol. 10, pp. 198–199.
Andrievskii, R.A., Kravchenko, S.E., and Shilkin, S.P., Preparation and some properties of ultrafine zirconium boride and titanium boride powders, Inorg. Mater., 1995, vol. 31, no. 8, pp. 965–968.
Hermann, W.A., Denk, M., and Schener, W., Cyclische Metalamide flüchtige Tetrahydroborat Komplexe von Titan und Zirconium, J. Organomet. Chem., 1993, vol. 444, no. 1, pp. 21–24.
Kravchenko, S.E., Torbov, V.I., and Shilkin, S.P., Nanosized zirconium diboride: Synthesis and properties, Russ. J. Inorg. Chem., 2011, vol. 56, no. 4, pp. 506–509.
Chen, L., Gu, Y., Chi, L., et al., Synthesis and oxidation of nanocrystalline HfB2, J. Alloys Compd., 2004, vol. 368, pp. 353–356.
Kim, J.W., Shim, J.H., Ahn, J.P., et al., Mechanical synthesis and characterization of TiB2 and VB2 nanopowders, Mater. Lett., 2008, vol. 62, pp. 2461–2464.
Chen, L., Qian, Y., Chi, L., Yang, Z., and Ma, J., A facile one-step route to nanocrystalline TiB2 powders, Mater. Res. Bull., 2004, vol. 39, pp. 609–613.
Volkova, L.S., Shul’ga, Yu.M., and Shilkin, S.P., Synthesis of nano-sized titanium diboride in a melt of anhydrous sodium tetraborate, Russ. J. Gen. Chem., 2012, vol. 82, no. 5, pp. 819–821.
Kravchenko, S.E., Torbov, V.I., and Shilkin, S.P., Preparation of titanium diboride nanopowder, Inorg. Mater., 2010, vol. 46, no. 6, pp. 614–616.
Chen, L., Gu, Y., Qian, Y., et al., A reduction-boronation route to nanocrystalline titanium diboride, Solid State Commun., 2004, vol. 130, pp. 231–233.
Semenenko, K.N., Shilkin, S.P., Burnasheva, V.V., et al., Reactions of CeFe2-LaFe2 alloys with nitrogen in the presence of hydrogen, Zh. Obshch. Khim., 1983, vol. 53, no. 5, pp. 961–966.
Fokin, V.N., Fokina, E.E., and Shilkin, S.P., Synthesis of coarsely crystalline metal hydrides, Russ. J. Gen. Chem., 1996, vol. 66, no. 8, pp. 1210–1212.
Semenenko, K.N., Shilkin, S.P., Burnasheva, V.V., et al., Reactions of some intermetallic compounds between rare-earth and iron-group metals with nitrogen in the presence of hydrogen, Zh. Obshch. Khim., 1987, vol. 57, no. 4, pp. 729–732.
Eksperimental’nye metody v adsorbtsii i molekulyarnoi khromatografii (Experimental Techniques in Adsorption and Molecular Chromatography), Kiselev, A.V. and Dreving, V.P., Eds., Moscow: Mosk. Gos. Univ., 1973.
Andrievskii, R.A. and Spivak, I.I., Prochnost’ tugoplavkikh soedinenii i materialov na ikh osnove (Strength of Refractory Compounds and Related Materials), Chelyabinsk: Metallurgiya, 1989.
Ilyushchenko, N.G., Anfinogenov, A.I., and Shurov, N.I., Vzaimodeistvie metallov v ionnykh rasplavakh (Interaction of Metals in Ionic Melts), Moscow: Nauka, 1991.
Dymova, T.N., Eliseeva, N.G., and Mikheeva, V.I., Thermoanalytical study of sodium borohydride and related substances, Zh. Neorg. Khim., 1967, vol. 12, no. 9, pp. 2317–2320.
Aleshin, V.G., Kharlamov, A.N., and Chudinov, M.G., Surface condition of refractory compounds studied by X-ray photoelectron spectroscopy, Izv. Akad. Nauk SSSR, Neorg. Mater., 1979, vol. 15, no. 4, pp. 672–676.
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Original Russian Text © L.S. Volkova, S.E. Kravchenko, I.I. Korobov, A.M. Kolesnikova, N.N. Dremova, A.G. Burlakova, G.V. Kalinnikov, S.P. Shilkin, 2013, published in Neorganicheskie Materialy, 2013, Vol. 49, No. 11, pp. 1173–1177.
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Volkova, L.S., Kravchenko, S.E., Korobov, I.I. et al. Preparation of titanium diboride nanopowders of different particle sizes. Inorg Mater 49, 1086–1090 (2013). https://doi.org/10.1134/S0020168513110137
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DOI: https://doi.org/10.1134/S0020168513110137