Nano-sized Fe particles were synthesized by Chemical Vapor Condensation (CVC) Process using the precursor of iron carbonyl (Fe(CO)5) as the source. We investigated the microstructures, magnetic properties of the Fe nanoparticles and their oxidation behavior during annealing systematically by means of HRTEM, DTA-TG, Mössbauer spectroscopy. The prepared particle was nearly spherical shape and core-shell type structure. The magnetic states of Fe nanoparticles changed from superparamagnetism to ferromagnetism with the particle size and microstructure. Oxidation heat treatment leads to the successive appearance of oxide phases.