Study On The Preparation, The Purification And Characterization Of A Novel Higher Fullerene

Higher fullerenes were successfully prepared by the novel experiment method established and developed by our group, which is Pulsed Laser Ablation at the Interface of Target Submerged in Flowing Liquid(PLA-IT/AFL).In this investigation, Graphite or Fe or Ti or W was taken for solid target and aromatic hydrocarbon A or aromatic hydrocarbon B or alcohol was taken for flow-liquid, Catalyst was C. The productions were characterized in detail by LC-MS, TEM, HPLC, UV-Vis and so on. The results showed that several sort of fullerenes prepared by PLA-IT/AFL through taking graphite for solid target and aromatic hydrocarbon B for flow-liquid, and the content of C₉₈ in the productions was the highest. Taking metals such as Fe, Ti, W for solid target could not achieve fullerene.We in turns used alcohol, diethyl ether and toluene to extract the first production by Soxhlet-extraction method in the investigation. The fullerene mixture was purified by AlCl₃ saturated solution of toluene, AlCl₃ particles. The research showed that the effect was better with AlCl₃ particles than AlCl₃ saturated solution of toluene. Several purer components, which were C₂₄, C₃₈ and C₉₈, were extracted from fullerene mixture dissolved in the solution of alcohol and toluene by step-by-step precipitation and crystallization method. C₉₈ was the purest and most. The structure and property of C₉₈ were characterized by LC-MS, HREM, UV-Vis, FS, FI-IR and TG-DSC. The results indicated that the diameter of C₉₈ particles which were multilevel and irregular together was lnm, and the absorption intensity and the peak location of UV-Vis of C₉₈ changed in different solvent, the absorption curve of UV-Vis of C₉₈ in toluene was in the longer wavelength range, and the peak width at half height of the fluorescence emission peak of C₉₈ was 127nm, and thermo-stability of C₉₈ was better than C₆₀ in airbefore 335.9 °C afid worse than C6o after 335.9 °C , it started to be oxidized by O2 at 335.9 "C and generated CO, CO2, and the FI-IR absorption of C98 was at 1709.43, 1599.31, 1439.85, 1258.71, 1099.25, 1022.22, 879.00, 818.86 and 752.63cm'1 and the FI-IR absorption intensity of Cgg was a little weaker than C6o by ATR method.