Magnetic Co nanoparticles were synthesized by a chemical vapor condensation method using the precursor of cobalt carbonyl as the source under a flowing inert gas atmosphere. Characteristics of the resulting material were investigated systematically by means of X-ray diffraction, high resolution transmission electron microscopy, TEM, X-ray photoelectron spectroscopy, vibrating sample magnetometer and differential thermal analysis-thermogravimetry. A correlation between the preparation conditions and the resulting microstructure of the nanoparticles was studied.