Selective solution-phase generation and oxidation reaction of C60n− (n = 1,2) and formation of an aqueous colloidal solution of C60

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Abstract
The facile chemical methods for the selective solution-phase generation of C60n- (n = 1,2) and the preparation of an aqueous colloidal solution of C60 are reported. When C60 was treated with Al–Ni alloy or tin (or zinc powder or sodium hydrosulfite) in aqueous NaOH–THF or in aqueous NaOH–DMSO or DMF, C60- or C602- was produced selectively with no need for control of stoichiometry. The reaction products were characterized by ESI–MS, VIS–NIR, EPR and 13C NMR spectroscopies. It was found that C60n- (n = 1,2) was inert to water, but very sensitive to oxygen. The oxidation reaction of C602- with oxygen follows the sequence: C602-→C601- →C60, which is monitored by NIR absorption spectroscopy. When C60n- (n = 1,2) is oxidized in aqueous solution the C60 sol is formed, but in dry organic solvent black C60 powder is deposited. It was proved that the sol was composed of C60 by UV, FTIR and ESIMS. Transmission electron microscope analysis showed that the colloidal particles, ca. 10 nm in diameter, were non-crystalline and quite homogeneous.

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