In order to obtain mono-dispersed Fe NPs with high saturation magnetization, quantitative analysis method to investigate the growth dynamics of the Fe NPs synthesized by a conventional thermal decomposition method has been developed. As a result, fast nucleation process promotes formation of ~4 nm of initial nucleus with a non-equilibrium phase, resulting in low saturation magnetization. And slow particle growth with atomic-scaled surface precipitation mode (< 100 atoms/(min·nm 2 )) can form the growth layer on the surface of initial nucleus with high saturation magnetization (~190 emu/g Fe ) as an equilibrium a phase of Fe. Therefore, higher stabilization of small initial nucleus generated just after the injection of Fe(CO) 5 should be one of the key issues to achieve much higher M s of Fe NPs.