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Journal of Electron Microscopy 51:S97-S105 (2002)
© 2002 Oxford University Press

Full-length paper

TEM/EELS analysis of heat-treated carbon nanotubes: experimental techniques

Bryan W. Reed and Mehmet Sarikaya

Materials Science and Engineering, Roberts Hall, Box 352120, University of Washington, Seattle, WA 98195, USA

To whom correspondence should be addressed. E-mail: sarikaya{at}u.washington.edu

We describe the techniques used in a recent transmission electron microscope/electron energy-loss spectroscopy (TEM/EELS) investigation of the material properties of carbon nanotubes grown and heat-treated under various conditions. Essential considerations, such as choice of equipment, TEM and spectrometer conditions, sample preparation, control of radiation damage, data analysis, and reproducibility of results are all discussed. The combination of TEM imaging, core-loss EELS, and low-loss EELS provides detailed information about physical structure, chemical bonding, density, and electronic behaviour on a nanometre scale. The result is a much more complete profile of each material than would have been possible with a smaller set of techniques. Increasing the heat treatment temperature for a given batch of material is shown to increase the density, to increase the sp2/sp3 hybridization ratio, and for a temperature of 2150°C, to dramatically restructure the material. The procedures described are applicable to other nanotube materials and nanowires.

Keywords     nanotubes, EELS, TEM, nanowires, low-loss EELS, inner-shell EELS


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