electron microscopy
 

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Vanadium Oxide Nanotubes

Synthesis

Vanadium oxide nanotubes (VOx-NTs) are easily accessible as a pure product in gram quantities by a low-temperature, soft chemistry synthesis. Primary alkyl amines (CnH2n+1NH2 with n = 4 - 22) or alkyl diamines (H2N[CH2]nNH2 with n = 14 - 20) are reacted with a vanadium(V) alkoxide, and, after aging and a hydrothermal treatment at 180 C for about 1 week, the nanotubes are obtained in very high yield.

Morphology

The tubular structure can be already seen in high-resolution SEM images. The inner core appears to be empty while the tube walls show roll-up characteristics.

Structural Characterization
TEM investigations reveal that the tubes have an empty core and that a layered builds up the tube walls.

TEM image of cross-sections (left). A tube consisting of concentric shells (upper left part) and a single-layer scroll (upper right part) are present. Vanadium map obtained by ESI (middle). The sites containing V (bright contrast) appear at the same sites as the dark contrast in the TEM image. Carbon map (right). C is present around the tubes and in their core due to the organic embedding material used for the cross-sectional preparation.

A simple structural model for the tube walls could be derived from these results: vanadium oxide layers between which the amine molecules are embedded form the walls. Information obtained in reciprocal space by X-ray and electron diffraction led to a decription of the nanotube structure by a cell with a tetragonal metric (a = 0.62 nm and c being equal to the inter-layer distance). However, one should consider that three-dimensional periodicity is not present in nanotubes due to the bending of the layers. Thus, their structure can only approximately be described in the usual crystallographic terms.

A structural model for the wall structure of the VOx-NTs was derived in relation to a new crystalline vanadate. The X-ray powder diffractogram calculated with this models matches well with the simulated one.

 

Selected Publications

Redox-Active Nanotubes of Vanadium Oxide
M.E. Spahr, P. Bitterli, R. Nesper, M. Müller, F. Krumeich, and H.-U. Nissen, Angew. Chem. Int. Ed. 37 (1998) 1263-1265 DOI

Morphology and Topochemical Reactions of Novel Vanadium Oxide Nanotubes
F. Krumeich, H.-J. Muhr, M. Niederberger, F. Bieri, B. Schnyder, and R. Nesper, J. Am. Chem Soc. 121 (1999) 8324-8331 DOI

Vanadium Oxide Nanotubes - a New Flexible Vanadate Nanophase
H.-J. Muhr, F. Krumeich, U.P. Schönholzer, F. Bieri, M. Niederberger, L.J. Gauckler, and R. Nesper, Adv. Mater. 12 (2000) 231-234 DOI

Low-Cost Synthesis of Vanadium Oxide Nanotubes via Two Novel Non-Alkoxide Routes
M. Niederberger, H.-J. Muhr, F. Krumeich, F. Bieri, D. Günther, and R. Nesper, Chem. Mater. 12 (2000) 1995-2000 DOI

Controlled Uptake and Release of Metal Cations by Vanadium Oxide Nanotubes
J.M. Reinoso, H.-J. Muhr, F. Krumeich, F. Bieri, and R. Nesper, Helv. Chim. Acta 83 (2000) 1724-1733 DOI

The Cross-Sectional Structure of Vanadium Oxide Nanotubes Studied by Transmission Electron Microscopy and Electron Spectroscopic Imaging
F. Krumeich, H.-J. Muhr, M. Niederberger, F. Bieri, and R. Nesper, Z. anorg. allg. Chem. 626 (2000) 2208-2216 DOI

The First Oxide Nanotubes with Alternating Inter-Layer Distances
Krishnan S. Pillai, F. Krumeich, H.-J. Muhr, M. Niederberger, and R. Nesper, Solid State Ionics 411-412 (2001) 185-190 DOI

Flexible V7O16 Layers as the Common Structural Element of Vanadium Oxide Nanotubes and a New Crystalline Vanadate
M. Wörle, F. Krumeich, F. Bieri, H.-J. Muhr, and R. Nesper, Z. anorg. allg. Chem. 628 (2002) 2778-2784 DOI

 

ETH Zürich | ETH chemistry department | ETH inorganic chemistry

modified: 15 June, 2015 by F. Krumeich | © ETH Zürich and the authors