The work described in this paper is directed towards the electrosynthesis of TTFCl0,77 as spherical nanoparticles by using amphiphilic molecules, behaving as growth-controlling agents. The morphology and the size distribution of the particles were analyzed using transmission electron microscopy and the resulting powders were characterized by infrared and Raman spectroscopy along with X-ray diffraction. In the presence of dodecylamine, electron micrographs evidenced spherical and relatively well-dispersed nanoparticles exhibiting a mean diameter of about 10 nm. However, in the presence of N-octylfurfurylimine, a mixture of nanoparticles and sticks were formed. The best results in terms of smallness of particles size and narrowness size distribution were obtained in the presence of 1-octanamine, N-(2-thienylmethylene). Spherical nanoparticles exhibiting sizes in the 4–12 nm range with an average size of about 8 nm were observed. The nanoparticles powder exhibited a room temperature conductivity of about 0.01 S.cm–1.