This thesis describes the development and application of techniques for the production, isolation and characterisation of fullerenes and carbon nanotubes, and the attempted production of endohedral fullerenes. A benchtop carbon arc reactor for the macroscopic production of these species was built. The construction and characterisation of this carbon are reactor is described. Experiments aimed at optimising the productivity of the reactor by varying the operating conditions are described in relation to possible fullerene formation schemes. These included the effect of experimental variables such as reactor buffer gas pressure, discharge current, internal dimensions, and graphite electrode size on fullerene formation. The use of graphite electrodes packed with a possible fullerene precursor molecule, tri-indane, was also investigated as a means of probing fullerene formation mechanisms and increasing the quantity of fullerenes produced. A wide range of techniques for the extraction of fullerene rich soot and for chromatographic separation and mass spectrometric characterisation of the resulting fullerenes have been investigated. A high yield extraction protocol is described involving preliminary large scale separation of fullerenes by competitive complexation with AlCl<SUB>3</SUB>. Chromatographic studies led to the development of a novel stationary phase for separation of fullerenes using high performance liquid chromatography (HPLC).The characterisation of this stationary phase using on-line particle beam mass spectrometry is described. The change in enthalpy for adsorption of C<SUB>60</SUB> and C<SUB>70</SUB> on this stationary phase have been experimentally determined. A linear relationship between molecular weight and chromatographic retention time has also been established for fullerenes eluting from such a column.
| Identifer | oai:union.ndltd.org:bl.uk/oai:ethos.bl.uk:657642 |
| Date | January 1997 |
| Creators | McQuillan, Robert James |
| Publisher | University of Edinburgh |
| Source Sets | Ethos UK |
| Detected Language | English |
| Type | Electronic Thesis or Dissertation |
| Source | http://hdl.handle.net/1842/11157 |
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