FeSx nanoparticles were synthesized by the chemical vapor condensation (CVC) process using the pyrolysis of iron pentacarbonyl (Fe(CO)5) and sulfur (S). The influence of CVC parameter on the formation of nanoparticle and size distribution was studied. The synthesized nanoparticles consisting of FeS, FeS2 and Fe2O3 were nearly spherical shape and 5~40 nm in mean diameter. Obtained particles were studied by applying the field emission scanning electron microscopy (FESEM) and high resolution transmission electron microscopy (HRTEM) and X-ray diffraction (XRD) methods. Electrochemical properties of the electrode fabricated with synthesized nanoparticles were evaluated.