Abstract
Single crystalline nanorods (15–200 nm in diameter and hundreds nanometers in length) have been formed on the carbon-covered W wires by simple electric heating under a vacuum of 5 × 10-4 Pa. The chemical composition and crystalline structure of the nanorods were carefully investigated by various characterization techniques such as scanning electron microscopy, transmission electron microscopy, Raman spectroscopy, energy dispersive x-ray spectroscopy and electron energy loss spectroscopy. After ruling out any possible existence of carbon nanotubes (CNTs), tungsten carbide, W-Fe alloying, and formation of other types of tungsten oxides, monoclinic W18O49 phase has been well identified. The mechanism of nanorod formation of sub-tungsten oxide (~WO2.7 compared to WO3) will be discussed in relation to the sample preparation conditions.
Similar content being viewed by others
References
E.B. Franke, C.L. Trimble, J.S. Hale, M. Schubert, and J.A. Woollam: Infrared switching electrochromic devices based on tungsten oxide. J. Appl. Phys. 88, 5777 (2000).
J.L. Solis, A. Hoel, V. Lantto, and G.G. Granqvist: Infrared spectroscopy study of electrochromic nanocrystalline tungsten oxide films made by reactive advanced gas deposition. J. Appl. Phys. 89, 2727 (2001).
L. Meda, R.C. Breitkopf, T.E. Haas, and R.U. Kirss: Investigation of electrochromic properties of nanocrystalline tungsten oxide thin film. Thin Solid Films 402, 126 (2002).
K.H. Lee, Y.H. Fang, W.J. Lee, J.J. Ho, K.H. Chen, and K.S. Liao: Novel electrochromic devices (ECD) of tungsten oxide (WO3) thin film integrated with amorphous silicon germanium photodetector for hydrogen sensor. Sens. Actuators B 69, 96 (2000).
M. Boulova, A. Gaskov, and G. Lucazeau: Tungsten oxide reactivity versus CH4, CO and NO2 molecules studied by Raman spectroscopy. Sens. Actuators B 81, 99 (2001).
G.R. Bamwenda and H. Arakawa: The visible light induced photocatalytic activity of tungsten trioxide powders. Appl. Catal. A 210, 181 (2001).
F.B. Li, G.B. Gu, X.J. Li, and H.F. Wan: Preparation, characterization and photo-catalytic behavior of WO3/TiO2 nanopowder. Acta Phys.—Chim. Sinica 16, 997 (2000).
J. Hao, S.A. Studenikin, and M. Cocivera: Transient photoconductivity properties of tungsten oxide thin films prepared by spray pyrolysis. J. Appl. Phys. 90, 5064 (2001).
E.K.H. Salje: Polarons and bipolarons in tungsten oxide, WO3-x. Eur. J. Solid State Inorg. Chem. 31, 651 (1994).
A. Aird, M.C. Domeneghetti, F. Mazzi, V. Tazzoli, and E.K.H. Salje: Sheet superconductivity in WO3-x: Crystal structure of the tetragonal matrix. J. Phys. Condens. Matter 10, L569 (1998).
M-I. Baraton, L. Merhari, H. Ferkel, and J-F. Castagnet: Comparison of the gas sensing properties of tin, indium and tungsten oxides nanopowders: Carbon monoxide and oxygen detection. Mater. Sci. Eng. C 19, 315 (2002).
J.L. Solis, S. Saukko, L. Kish, C.G. Granqvist, and V. Lantto: Semiconductor gas sensors based on nanostructured tungsten oxide. Thin Solid Films 391, 255 (2001).
S.T. Li and M.S. El-Shall: Synthesis and characterization of photochromic molybdenum and tungsten oxide nanoparticles. Nanostruct. Mater. 12, 215 (1999).
Y.Q. Zhu, W. Hu, W.K. Hsu, M. Terrones, N. Grobert, J.P. Hare, H.W. Kroto, D.R.M. Walton, and H. Terrones: Tungsten oxide tree-like structures. Chem. Phys. Lett. 309, 327 (1999).
Z. Liu, Y. Bando, and C. Tang: Synthesis of tungsten oxide nanowires. Chem. Phys. Lett. 372, 179 (2003).
Y. Koltypin, S.I. Nikitenko, and A. Gedanken: The sonochemical preparation of tungsten oxide nanoparticles. J. Mater. Chem. 12, 1107 (2002).
W.B. Hu, Y.Q. Zhu, W.K. Hsu, B.H. Chang, M. Terrones, N. Grobert, H. Terrones, J.P. Hare, H.W. Kroto, and D.R.M. Walton: Generation of hollow crystalline tungsten oxide fibres. Appl. Phys. A 70, 231 (2000).
R. Diehl, G. Brandt, and E. Salje: The crystal structure of triclinic WO3. Acta Crystallogr. B 34, 1105 (1978).
E. Salje and K. Viswanathan: Physical properties and phase transitions in WO3. Acta Crystallogr. A 31, 356 (1975).
A.J.H. Kim and K.L. Kim: A study of preparation of tungsten nitride catalysts with high surface area. Appl. Catal. A 181, 103 (1999).
A. Aird and E.K.H. Salje: Sheet superconductivity in twin walls: Experimental evidence of WO3-x. J. Phys. Condens. Mater. 10, L377 (1998).
Y.T. Zhu and A. Manthiram: New route for the synthesis of tungsten oxide bronzes. J. Solid State Chem. 110, 187 (1994).
A.A. Mohammad and M. Gillet: Phase transformations in WO3 thin films during annealing. Thin Solid Films 408, 302 (2002).
K. Viswanathan, K. Brandt, and E. Salje: Crystal structure and charge carrier concentration of W18O49. J. Solid State Chem. 36, 45 (1981).
M.M. Dobson and R.J.T. Tilley: A new pseudo-binary tungsten oxide, W17O47. Acta Crystallogr. B 44, 474 (1988).
J.M. Berak and M.J. Sienko: Effect of oxygen-deficiency on electrical transport properties of tungsten trioxide crystals. J. Solid State Chem. 2, 109 (1970).
R.R. Schlittler, J.W. Seo, J.K. Gimzewski, C. Durkan, M.S.M. Saifullah, and M.E. Welland: Single crystals of singlewalled carbon nanotubes formed by self-assembly. Science 292, 1136 (2001).
M. Chrisholm, Y. Wang, A.R. Lupini, G. Eres, A.A. Puretzky, B. Brinson, A.V. Melechko, D.B. Geohegan, H. Cui, M.P. Johnson, S.J. Pennycook, D.H. Lowndes, S. Arepalli, C. Kittrell, S. Sivaram, M. Kim, G. Lavin, J. Kono, R. Hauge, and R.E. Smalley: Comment on “Single crystals of single-walled carbon nanotubes formed by self-assembly”. Science 300, 1236b (2003).
M.E. Welland, C. Durkan, M.S.M. Saifullah, J.W. Seo, R.R. Schlittler, and J.K. Gimzewsk: Response to Comment on “Single crystals of single-walled carbon nanotubes formed by selfassembly”. Science 300, 1236c (2003).
N. Braidy, M.A. El Khakani, and G.A. Botton: Single-wall carbon nanotubes synthesis by means of UV laser vaporization. Chem. Phys. Lett. 354, 88 (2002).
C. Journet, W. Maser, P. Bernir, A. Loiseau, M. Delachapelle, S. Lefrant, P. Deniard, R. Lee, and J. Fischer: Large-scale production of single-walled carbon nanotubes by the electric-arc technique. Nature 388, 756 (1997).
O. Pyper, A. Kaschner, and C. Thomsen: In situ Raman spectroscopy of the electrochemical reduction of WO3 thin films in various electrolytes. Sol. Energy Mater. Sol. Cell. 71, 511 (2002).
J. Purans, A. Kuzmin, Ph. Parent, and C. Laffon: Study of the electronic structure of rhenium and tungsten oxides on the O K-edge. Physica B. Condens. Matter 259, 1157 (1999).
J. Purans, A. Kuzmin, Ph. Parent, and C. Laffon: X-ray absorption study of the electronic structure of tungsten and molybdenum oxides on the O K-edge. Electrochem. Acta 46, 1973 (2001).
D.W. Bullet: Bulk and surface electron states in WO3 and tungsten bronzes. J. Phys. C 16, 2197 (1983).
P. Villars and L.D. Calvert: Person’s Handbook of Crystallographic Data for Intermetallic Phases (ASM International, Materials Park, OH, 1991), p. 4792.
E. Lassner and W.D. Schubert: Tungsten: Properties, Chemistry, Technology of the Element, Alloys, and Chemical Compounds (Kluwer Academic/Plenum Publishers, New York, NY, 1999), p. 85–176.
Binary Alloy Phase Diagram, 2nd ed., edited by T.B. Massalski (ASM International, Metals Park, OH, 1990).
Author information
Authors and Affiliations
Rights and permissions
About this article
Cite this article
Guo, D.Z., Yu-Zhang, K., Gloter, A. et al. Synthesis and characterization of tungsten oxide nanorods. Journal of Materials Research 19, 3665–3670 (2004). https://doi.org/10.1557/JMR.2004.0469
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1557/JMR.2004.0469