Paul R. Birkett

Hydrogenation of [60]fullerene using a novel chemical vapour modification (CVM) method

The radical hydrogenation of [60]fullerene has been investigated using a novel chemical vapour modification (CVM) technique. Hydro[60]fullerenes were collected as solid products from the reaction of hydrogen atoms, which are formed at a hot filament surface, with sublimed [60]fullerene. The CVM process parameters such as the time of reaction, hydrogen pressure, filament and substrate temperatures have been optimised. The highest yield of C3v symmetric C60H18 was obtained when a filament temperature of not, vert, similar1900 K, which results in a substrate holder temperature of not, vert, similar960 K, a reaction time of 30 min and a hydrogen pressure of 20 Torr were used.

Functionalization of [60]Fullerene Using a Novel Chemical Vapor Modification Method

Abstract Gas phase reactions of [60]fullerene with hydrogen atoms and/or methyl radicals have been performed by hot filament chemical vapor modification (CVM) to produce hydrogenated and/or methylated [60]fullerene. The CVM process parameters such as the time of reaction, pressure, and percentage of methane diluted in hydrogen have been varied so as to obtain the addended fullerene reaction products. Mass spectrometry and 1H NMR techniques were used to characterize the reaction products obtained.

The synthesis of high-content fullerene functionalised polymers through the controlled addition of an amine-tagged fullerene derivative

A method has been developed for synthesising a series of soluble C60 containing polymers which have the characteristic photophysical properties of monosubstituted-fullerene derivatives. The strategy employed required that first a suitably derivatised mono-fulleropyrrolidine was prepared and characterised which was then subsequently reacted with an acryloyl chloride functionalised polymer. The amino group of the fulleropyrrolidine reacts with the acyl chloride functional groups of the polymer forming an amide bond. This approach enabled the preparation of several soluble fullerene/acrylic polymers with a controlled and high covalently bonded fullerene content. The resulting fullerene derivatised methacrylate polymers were characterised by UV, infrared and gel permeation chromatography.

Methylation of C60 Using the Modified Hot Filament Chemical Vapour Deposition Method

The methylation of C60 was performed via a gas‐phase reaction in a CH4/H2 atmosphere using a modified hot filament chemical vapour deposition (HFCVD) method. Pressures were varied from 20–45 torr, substrate temperatures set at 690°C and reaction times up to 15 minutes. High‐resolution matrix‐assisted laser desorption ionisation (MALDI) mass spectrometry was used to determine the synthetic route of the methylated products through accurate mass measurements. The analysis established the production of C60H18‐2n(H,CH3)n (n = 1–3). Collision‐induced dissociation experiments confirmed a maximum of 18 ligands possible to the C60 cage. The formation of carbon spheres with diameters up to 25 µm on the surface of the tungsten filament subsequent to HFCVD is also reported.