Filling Single Wall Carbon Nanotubes with Metal Chloride and Metal Nanowires and Imaging with Scanning Transmission Electron Microscopy

Nanowires of magnetic metals (Ho, Gd) have been synthesized inside the hollow interior of single wall carbon nanotubes by the sealed-tube reaction. Amongst the d- and f-series metal chlorides investigated in this study, HoCl3 and GdCl3 fill the SWNTs to a significantly higher extent than FeCl2 and CoCl2. HoCl3 and GdCl3 nanowires have been transformed into the respective metal nanowires via the reduction of the chloride nanowires. The nanowires have been imaged using high-resolution transmission electron microscopy and scanning transmission electron microscopy (STEM). X-ray energy dispersive spectroscopy carried out in conjunction with STEM confirmed the presence of metal chloride and metal nanowires

Structure and properties of C\u3csub\u3e60\u3c/sub\u3e@SWNT

Our recent achievement of high-yield C60@SWNT synthesis facilitates characterization by various techniques, including selected area electron diffraction (SAD) and Raman spectroscopy. The obtained SAD patterns show that interior C60 molecules sit on a simple 1-D lattice having a parameter of 1.00 nm. Simulated SAD patterns and real-space measurements both support this determination and do not indicate a lattice with a more complex basis, e.g. a dimer basis. Empty and bulk-filled SWNTs (22%, 56%, and 90% yields), each subjected to identical processing steps, were examined by room temperature Raman spectroscopy. Systematic differences are seen between the spectra of filled and unfilled SWNTs, particularly with respect to the G- and RBM-bands of the nanotubes. We present a possible explanation for this behavior

Reproducible synthesis of C\u3csub\u3e60\u3c/sub\u3e@SWNT in 90% yields

In previous works, we have shown our discovery of C60@SWNT and first described the general mechanism of filling, which involves the vapor phase transport of C60 molecules to openings in the SWNTs\u27 walls. Here, we discuss the high-yield synthesis of C60@SWNT by refinements to our method. Yields are measured by a calibrated weight uptake technique, a methodology that is not subject to many of the potential pitfalls inherent to other techniques that have been applied. At certain processing conditions, yields exceeding 90% were obtained and corroborated by transmission electron microscopy. From our data, we determine the parameters most important for creating endohedral SWNT supramolecular assemblies by the vapor phase method. Our results pave the way for successful single-tube measurements and for high-yield filling with non-fullerenes

Processing of single wall carbon nanotubes and implications for filling experiments

Single wall carbon nanotubes (SWNTs) have been processed in different schemes to get clean material for use in various filling experiments. The SWNTs synthesized by different methods require different processing schemes, and this is presumably due to heterogeneous nature of the various contaminants present along with the carbon nanotubes. For the pulsed laser synthesized SWNTs, a combination of nitric acid, hydrogen peroxide and hydrochloric acid treatment gives best results and the purified SWNTs give best ever filling fraction for fullerene, C60 of ~90%. The processing improves the surface cleanliness of SWNTs, in turn giving greater access for the target molecules, and hence the higher filling fraction. For the carbon arc produced SWNTs, air oxidation followed by treatment with nitric acid has been found to work best and the processed SWNTs have been used for filling experiments with metal chlorides. Both these processing schemes still leave a small fraction of catalyst impurities in the final material, thus the material quality of filled material and hence its properties depend on the processed material used for the filling experiments