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Although it is some five years since fullerenes were extracted in macroscopic quantities from the black, superficially amorphous sooty deposits produced by a carbon arc under helium, little is known in detail about the structure of the deposit or its electrical and magnetic properties. Here we provide evidence that this deposit, known as fullerene soot, is composed of defective networks of carbon atoms which do not have all valencies satisfied. We have studied these soots, before and after thermal annealing, using x-ray and electron diffraction, electron spin-resonance (ESR) spectroscopy, infra-red transmission and measurements of electrical conductivity. We find that localized states associated with such dangling bonds are removed from the soot on annealing and this process is accompanied by an ordering transition which modifies the electrical and magnetic properties. The fullerene soot particles appear to be encapsulated aggregates of highly defective carbon `onions'. Such metastable defective networks undergo a subtle ordering processes upon heat treatment which is accompanied by a rise in the electrical conductivity and a loss of paramagnetism due to the elimination of unsatisfied carbon atom valencies. Electrical conductivity and infra-red transmission measurements indicate that the centre of these `onions' is graphitic, with metallic properties. The temperature dependence of the electrical conductivity suggests that charge transport in both annealed and unannealed materials occurs by tunnelling between metallic islands in the sample. The ESR linewidth, arising from the spin centres in fullerene soots, is not significantly changed by exposure to oxygen. This suggests that the free radical centres in fullerene soots are extremely efficiently isolated from the atmosphere - presumably by encapsulation. This behaviour contrasts with that of amorphous carbons prepared by thermal decomposition of organic materials (chars). The ESR g-factors of the fullerene soots are lower than those of chars, which suggests that the radicals in fullerene soots have strong sigma character due to unsatisfied -type valencies. In this paper, a plausible structure and associated annealing mechanism for the fullerene soot is presented based on these experimental observations. .

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An autoclave cell has been designed for performing time‐resolved neutron diffraction analyses of the dynamic processes occurring during hydrothermal syntheses under hostile (corrosive and explosive) conditions: such conditions include those of hot NaOH/NaOD solutions and pressurized steam. The cell is also capable of measuring differential pressures and accurate sample temperatures as required for the study of reactions which are temperature sensitive. The cell is described and examples of its successful use are given illustrating the synthesis of basic zeolites and a layered calcium silicate hydrate. This technique has considerable potential for studying a variety of synthesis processes of industrial importance, such as in the production of catalysts and the hydration of cements.

Common soots are disordered carbonaceous materials containing several per cent of heteroatoms. A question of some importance is to what extent pure carbon networks dominate the properties of common soots. Here, we report the results of a comparative study of fullerene soots which are a form of pure partially ordered carbon and those formed from flaming polystyrene combustion which contain a few per cent of oxygen atoms, using electron diffraction, electron spin resonance (ESR), infra-red transmission and measurements of electrical conductivity. It has been found that despite some important characteristic differences, the annealed fullerene soot and flaming polystyrene soot have a number of important structural, electrical and magnetic features in common, provided that the flame and annealing temperatures are the same. This suggests that the graphitic layer and fullerene related tubular structures found in these materials dominate the electrical properties of these soots regardless of the presence of small quantities of heteroatoms in the soot derived from the flaming combustion of polystyrene.