Synthesis of C and CN x Nanotubes, Using the Aerosol Method
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Synthesis of C and CNx Nanotubes, Using the Aerosol Method M. Glerup*1, M. Castignolles1,2, M. Holzinger1, H. Kanzow1,3, A. Loiseau2 and P. Bernier1 1 Groupe de Dynamique des Phases Condensées (UMR5581),Université Montpellier II, Place E. Bataillon, 34095 Montpellier, France 2 Laboratoire d’Etude des Microstructures, ONERA-CNRS (UMR104), 29, av. de la Division Leclerc, BP72, 92322 Châtillon, France 3 New address: ContiTech Antriebsysteme, 30165 Hannover, Germany *corresponding author: [email protected] ABSTRACT Here we will present the state-of-the-art of the aerosol synthesis method. We demonstrate the reliability of this method by showing that the method can be successfully used for the synthesis of C and CNx multi walled nanotubes. For characterization, scanning- (SEM) and high resolution transmission electron microscopy (HRTEM) imaging have been carried out. The N/C ratio is determined using Electron Energy Loss Spectroscopy (EELS) combined with TEM. INTRODUCTION A lot of attention has been given to the research of nanotubes since their discovery in 1991 [1] especially because of their unique electronic and mechanical properties. Nanotubes are expected to bring breakthroughs in the electronic and mechanical engineering of materials. Thus, for the successful use of nanotubes for industrial application, the efficient and well-controlled synthesis of nanotubes is a key issue. The electronic properties of undoped carbon nanotubes vary between semi-conducting and metallic, depending on their helicity [2]. A way to modulate the electronic properties of nanotubes is by doping them with other chemical elements, as for example nitrogen. N-doped nanotubes are found to be exclusively metallic conductors [3, 4]. Doping carbon nanotubes can be done in two essential different ways, either by post reactions of carbon nanotubes (CNTs) with a nitrogen containing compound, or by the direct synthesis of Ndoped CNTs. Here we will demonstrate that the aerosol method can be used for the synthesis of carbon nanotubes. By using aerosols with a well-defined size we can predict the size of the active catalyst. At last it will be shown that the aerosol method can be used with a great success for the direct synthesis of nitrogen doped tubes. EXPERIMENTAL A sketch of the set-up is given in Fig. 1. An aerosol injector is directly connected to a high temperature furnace. The aerosol injector produces aerosol with a well-defined size. The gas mixture used for the production of the aerosols consists of hydrogen and argon. For the synthesis of multi walled carbon nanotubes tetrahydrofuran (THF) is used as the carbon source and cobalt nitrate as the catalyst precursor [5]. The experiments are carried out at 700°C. For the nitrogen-doped nanotubes, a mixture of acetonitril and tetrahydrofuran was used, and with [Fe(acac)3] as the catalyst precursor. These experiments were carried out at 950°C. The exact details for the experimental set-up is given in Ref. [6].
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