We have found that metal/fullerene adduct ions of the C<sub>60</sub> and C<sub>70</sub> fullerenes can be formed with silver, gold, rhodium, and palladium by argonion bombardment of fullerenes deposited on a metal substrate, with the use of a Time-of-Flight Secondary Ion Mass Spectrometer (TOF-SIMS). The <i>bis</i> and <i>tris</i> metal/fullerene adducts formed include: Ag(C<sub>60</sub>)<sub>2</sub><sup>+</sup>, AgC<sub>60</sub>C<sub>70</sub><sup>+</sup>, Ag(C<sub>70</sub>)<sub>2</sub><sup>+</sup>, Ag(C<sub>60</sub>)<sub>3</sub><sup>+</sup>, Ag(C<sub>60</sub>)<sub>2</sub>C<sub>70</sub><sup>+</sup>, AgC<sub>60</sub>(C<sub>70</sub>)<sub>2</sub><sup>+</sup>, and Rh(C<sub>60</sub>)<sub>2</sub><sup>+</sup>. In addition, the monomeric adducts AgC<sub>60</sub><sup>+</sup>, AgC<sub>70</sub><sup>+</sup>, AuC<sub>60</sub><sup>+</sup>, AuC<sub>70</sub><sup>+</sup>, RhC<sub>60</sub><sup>+</sup>, RhC<sub>70</sub><sup>+</sup>, and PdC<sub>60</sub><sup>+</sup> also have been detected. Samples prepared with a raw soot extract gave higher yields of metal/fullerene adducts in TOF-SIMS than those prepared with purified fullerenes. This result may indicate the presence of a matrix component in the raw soot which enhances the formation of fullerene/metal adducts. Spectra obtained from the raw soot show peaks at every 24 daltons corresponding to even-numbered carbon clusters. These peaks occur as low as 600 daltons (C<sub>50</sub>) and as high as 3000 (C<sub>250</sub>).

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