Production of short carbon nanotubes with open tips by ball milling

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Abstract

Short multi-wall carbon nanotubes can be obtained by ball milling. The average length of the ball milled carbon nanotubes, synthesised by decomposition of acetylene on different types of supported metal catalysts, is ca. 0.8 μm. The cleavage was caused by the collision between one agate ball and the nanotube powder contained in an agate mortar.

Introduction

Since the discovery of nanotubes in 1991 by Iijima [1], this new form of carbon has aroused interest in their fabrication [2] (arc discharge, catalytic decomposition of hydrocarbons, laser ablation…) and also their properties (Young modulus [3], adsorption process [4], electric properties [5], [6], [7]). The application fields are various: field emission [8], electric conductivity [9], hydrogen storage [10], [11], [12], [13], molecular sieves [14], etc.

As far as the latter two applications are concerned, short nanotubes with open ends are required to overpass the diffusion limitation. Recently, interest has focussed on producing small nanotubes (shorter than 1 μm). The different methods proposed to cut nanotubes are ultrasound power [15], [16], [17] and STM voltage [18]. Nevertheless, these techniques are limited to producing milligram scale quantities. Ball milling has already been utilised for production of nanoparticles [19] or nanoporous carbon [20], but also for curving nanotubes [21]. In this paper, we present a new and simple technique to obtain short nanotubes in gram scale quantities with open tips by the ball milling process, starting from long multi-wall carbon nanotubes. The cleavage was followed by TEM as a function of the ball milling time. A cutting mechanism of the nanotubes based on the collision between one agate ball and the nanotube powder contained in an agate mortar is proposed.

Section snippets

Production of the long carbon nanotubes

Multi-wall carbon nanotubes were prepared by catalytic decomposition of acetylene using Co or Co/Fe catalyst supported on NaY zeolite. Catalyst preparation has been already described elsewhere [22], [23], [24]. We used the impregnation method with a concentration of 5 wt% for Co alone and 2.5/2.5 wt% for Co/Fe. The production of nanotubes was carried out at 700°C during 1 h using acetylene flow of 30 and 300 ml/min of N2 as carrier gas. Nanotubes synthesised on Co/NaY and Co/Fe/NaY have an

Results and discussion

From TEM observations, it was possible to measure nanotube length and distribution. The evolution of the average nanotube length as a function of the ball milling time was determined for the two types of nanotubes. Structural characteristics of the nanotubes were also studied and a nanotube-cleavage model was elaborated.

Conclusions

The ball milling process is a good method to obtain short (<1 μm) multi-wall carbon nanotubes with open tips. The cleavage of catalytically synthesised multi-wall carbon nanotubes (either crude or purified) gives short nanotubes. The average length varies from 0.7 to 0.9 μm. Moreover, homogeneous nanotube samples are obtained and no other form of carbon is generated during ball milling (even after 120 h of processing). The nanotube final length depends mainly on the characteristics of the ball

Acknowledgements

N. Pierard and I. Willems gratefully acknowledge support from FRIA. The authors thank the Belgian Programme on Inter University Poles of Attraction initiated by the Belgian State, Prime Minister's Office for Scientific, Technical and Cultural Affairs (OSTC-PAI-IUAP No. 4/10 on Reduced Dimensionality Systems) for financial support.

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