A significant and versatile approach was developed for perpendicularly aligning multiwall carbon nanotubes on diverse substrates suitable for layer-by-layer self-assembly. The multiwall carbon nanotubes (s-MWNTs) used were shortened with oxidation under ultrasonic and functionalized with acyl chloride in thionyl chloride (SOCl2) The monolayer of s-MWNTs perpendicularly grafted to the substrate was obtained by dipping the polyelectrolyte modifying substrate into a tetrahydrofuran Suspension of the functionalized s-MWNTs. The interaction proved to be stable and not liable to be affected by the ambience. Transmission electron microscopy and atomic force microscopy were used to examine the morphology of the MWNTs and s-MWNTs grafted on the substrates. Raman spectroscopy was applied to verify the existence of s-MWNTs for assembly, and Fourier transform infrared absorption spectra were used to investigate the interaction pattern between s-MWNTs and polyelectrolyte. The electrochemistry properties of the monolayer of s-MWNTs when the substrate was indium-tin oxide were studied. (c) 2004 Elsevier Inc. All rights reserved.