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Titanium nitride nanopowders produced via sodium reductionin liquid ammonia

Published online by Cambridge University Press:  31 January 2011

Hongmin Zhu*
Affiliation:
School of Metallurgical and Ecological Engineering, University of Science and Technology Beijing, Beijing 100083, People's Republic of China
*
a) Address all correspondence to this author. e-mail: hzhu@metall.ustb.edu.cn
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Abstract

Titanium nitride nanopowders were synthesized through a chemical reduction of titanium tetrachloride by sodium in liquid ammonia. The products of the reaction were the mixture of sodium chloride and titanium nitride nanopowders. The mixture was then separated by ammonia extraction. The nanopowders were heated under vacuum up to 1200 °C and were characterized by x-ray diffraction (XRD), transmission electron microscopy (TEM), Brunauer-Emmet-Teller (BET) surface area measurement, and chemical analysis. The results show that the product is nanocrystalline cubic phase TiN with Ti/N atomic ratio performed 1:1, and the surface area is from 20 to 50 m2 ·g−1 depending on the heating temperature. The particle sizes estimated by the TEM analysis correspond well with the results of the surface area measurements. The XRD pattern indicates that the crystal size grows with an increase in heating temperature.

Type
Articles
Copyright
Copyright © Materials Research Society 2009

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References

REFERENCES

1.Toth, L.E.: Transition Metal Carbides and Nitrides(Academic Press New York and London 1971)219Google Scholar
2.Wang, D.Z., Wang, X., Yang, G.Q., Liu, X.H., Jia, Y.B., Zhou, G., Li, G.F.: Phase and structures of nano-crystalline TiN films. J. Appl. Phys. 77, 2945 (1995)CrossRefGoogle Scholar
3.Ruhl, G., Frőschle, B., Ramn, P., Intemann, A., Pamler, W.: Deposition of titanium nitride/tungsten layers for application in vertically integrated circuit technology. Appl. Surf. Sci. 91, 382 (1995)Google Scholar
4.Il-seok, K., Kumta, P.N., Blomgren, G.E.: Si/TiN nanocomposites novel anode materials for Li-ion batteries. Electrochem. Solid-State Lett. 3, 493 (2000)Google Scholar
5.Wang, L., Wan, J., Chen, L., Yang, M., Zhu, H.: Consolidation of nano-sized TiN powders by spark plasma sintering. J. Am. Ceram. Soc. 89, 2364 (2006)CrossRefGoogle Scholar
6.Ananthapadmanabhan, P.V., Patrick, R.T., Zhu, W.X.: Synthesis of titanium nitride in a thermal plasma reactor. J. Alloys Compd. 287, 126 (1999)CrossRefGoogle Scholar
7.Nakagawa, Y., Grigoriu, C., Masugata, K., Jiang, W.H., Yatsui, K.: Synthesis of TiO2 and TiN nanosize powders by intense light ion-beam evaporation. J. Mater. Sci. 33, 529 (1998)Google Scholar
8.Vaidhyanathan, B., Agrawal, D.K., Roy, R.: Novel synthesis of nitride powders by microwave-assisted combustion. J. Mater. Res. 15, 974 (2000)CrossRefGoogle Scholar
9.Sato, T., Yasuda, S., Usuki, K., Yoshioka, T., Okuwaki, A.: Synthesis of titanium nitride by a spark-discharge method in ammonia. J. Mater. Sci. 31, 2495 (1996)Google Scholar
10.Zhang, F., Kaczmarek, W.A., Lu, L.: Formation of titanium nitrides via wet reaction ball milling. J. Alloys Compd. 307, 249 (2000)CrossRefGoogle Scholar
11.Nishikiori, T., Nohira, T., Goto, T., Ito, Y.: Acceleration of electrochemical titanium nitride growth by addition of LiH in a molten LiCl-KCl-Li3N systems. Electrochem. Solid-State Lett. 2, 278 (1999)CrossRefGoogle Scholar
12.Herle, P.S., Hegde, M.S., Vasathacharya, N.Y., Philip, S.: Synthesis of TiN, VN, and CrN from ammonolysis of TiS2. J. Solid State Chem. 134, 120 (1997)Google Scholar
13.Ren, R.M., Yang, Z.G., Shaw, L.L.: Nanostructured TiN powder prepared via an integrated mechanical and thermal activation. Mater. Sci. Eng., A 286, 65 (2000)Google Scholar
14.Clément, F., Bastians, P., Grange, P.: Novel low-temperature synthesis of titanium nitride: Proposal for cyanonitridation mechanism. Solid State Ionics 101-103, 171 (1997)CrossRefGoogle Scholar
15.Hu, J.Q., Lu, Q.Y., Tang, K.B., Yu, S.H., Qian, Y.T., Zhou, G.E., Liu, X.M.: Low-temperature synthesis of nano-crystalline titanium nitride via a benzene-thermal route. J. Am. Ceram. Soc. 83, 430 (2000)CrossRefGoogle Scholar
16.Nicholls, D.: Inorganic Chemistry in Liquid Ammonia(Elsevier Amsterdam, Netherlands 1979), p. 179Google Scholar
17.Zhu, H., Sadoway, D.R.: Synthesis of nanoscale particles of Ta and Nb3Al by homogeneous reduction in liquid ammonia. J. Mater. Res. 16, 2544 (2001)CrossRefGoogle Scholar
18.Cullity, B.D.: Elements of X-Ray Diffraction(Addison-Wesley Reading Mass., MA 1959)99Google Scholar