In this paper, the formation in situ of an electrodeposited film of (TBA(+))(n)(C-60(n-)) (n = 1 to 3) on a microelectrode and its voltammetric behavior have been studied. The method consists of electroreducing C-60 in a mixed solvent of acetonitrile and xylene (1:6 v/v) and a supporting electrolyte of 0.08 M TBAPF(6) at a potential sufficiently negative to generate C-60(3-) anion, followed by deposition of (TBA(+))(3)(C-60(3-)) on a microdisk electrode. Deposition conditions of the film and some of its characteristics were investigated. The standard surface electron-transfer rate constants k(0) and electron-transfer coefficient alpha of the two stripping reactions were determined.