Synthesis of carbon nanotube films by thermal CVD in the presence of supported catalyst particles. Part I: The silicon substrate/nanotube film interface

Magazine article, 2004

The interface between the silicon substrate and a carbon nanotube film grown by thermal CVD with acetylene (C2H2) and hydrogen at 750 or 900 °C has been characterized by high resolution and analytical transmission electron microscopy, including electron spectroscopic imaging. Silicon (0 0 2) substrates coated with a thin (2.8 nm) iron film were heat treated in the CVD furnace at the deposition temperature in a mixture of flowing argon and hydrogen whereby nanosized particles of (Fe,Si)3O4 formed. These particles were reduced to catalytic iron silicides with the α–(Fe, Si), α2–Fe2Si and α1–Fe2Si structures during CVD at 900 °C, and multi-wall carbon nanotubes grew from supported particles via a base-growth mechanism. A limited number of intermediate iron carbides, hexagonal and orthorhombic Fe7C3, were also present on the substrate surface after CVD at 900 °C. The reduction of the preformed (Fe, Si)3O4 particles during thermal CVD at 750 °C was accompanied by disintegration leading to the formation of a number of smaller (<5 and up to 10 nm) iron and silicon containing particles. It is believed that the formation of these small particles is a prerequisite for the growth of aligned multi-wall carbon nanotube films.