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Surface Composition of Carbon Nanotubes-Fe-Alumina Nanocomposite Powders: An Integral Low-Energy Electron Mo1ssbauer Spectroscopic Study

Gonzaga de Resende, Valdirene and De Grave, Eddy and Peigney, Alain and Laurent, Christophe Surface Composition of Carbon Nanotubes-Fe-Alumina Nanocomposite Powders: An Integral Low-Energy Electron Mo1ssbauer Spectroscopic Study. (2008) Journal of Physical Chemistry C, 112 (15). 5756-5761. ISSN 1932-7447

(Document in English)

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Official URL: http://dx.doi.org/10.1021/jp711679w


The surface state of carbon nanotubes-Fe-alumina nanocomposite powders was studied by transmission and integral low-energy electron Mo¨ssbauer spectroscopy. Several samples, prepared under reduction of the R-Al1.8-Fe0.2O3 precursor in a H2-CH4 atmosphere applying the same heating and cooling rate and changing only the maximum temperature (800-1070 °C) were investigated, demonstrating that integral low-energy electron Mo¨ssbauer spectroscopy is a promising tool complementing transmission Mössbauer spectroscopy for the investigation of the location of the metal Fe and iron-carbide particles in the different carbon nanotubenanocomposite systems containing iron. The nature of the iron species (Fe3+, Fe3C, R-Fe, ç-Fe-C) is correlated to their location in the material. In particular, much information was derived for the powders prepared by using a moderate reduction temperature (800, 850, and 910 °C), for which the transmission and integral low-energy electron Mössbauer spectra are markedly different. Indeed, R-Fe and Fe3C were not observed as surface species, while ç-Fe-C is present at the surface and in the bulk in the same proportion independent of the temperature of preparation. This could show that most of the nanoparticles (detected as Fe3C and/or ç-Fe-C) that contribute to the formation of carbon nanotubes are located in the outer porosity of the material, as opposed to the topmost (ca. 5 nm) surface. For the higher reduction temperatures Tr of 990 °C and 1070 °C, all Fe and Fe-carbide particles formed during the reduction are distributed evenly in the bulk and the surface of the matrix grains. The integral low-energy electron Mo¨ssbauer spectroscopic study of a powder oxidized in air at 600 °C suggests that all Fe3C particles oxidize to R-Fe2O3, while the R-Fe and/or ç-Fe-C are partly transformed to Fe1-xO and R-Fe2O3, the latter phase forming a protecting layer that prevents total oxidation.

Item Type:Article
Additional Information:Thanks to American Chemical Society editor. The definitive version is available at http://pubs.acs.org The original PDF of the article can be found at Journal of Physical Chemistry C website : http://pubs.acs.org/journal/jpccck
HAL Id:hal-03578175
Audience (journal):International peer-reviewed journal
Uncontrolled Keywords:
Institution:French research institutions > Centre National de la Recherche Scientifique - CNRS (FRANCE)
Université de Toulouse > Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE)
Université de Toulouse > Université Toulouse III - Paul Sabatier - UT3 (FRANCE)
Other partners > Universiteit Gent - UGENT (BELGIUM)
Laboratory name:
Deposited On:03 Jun 2009 13:21

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