Ultra-fine Fe2O3 nano-particles are synthesized using H-2/O-2 CO-axial diffusion flame with the state-of-the-art electro-spraying (e-spray) technique at atmospheric condition. Fe(CO)(5) is used as a precursor and the liquid phase Fe(CO)(5) is injected directly into the center of the flame using the electro-spraying method. The synthesized particle morphology sampled from the inside of flame is analyzed by TEM. The synthesized particles showed different crystal structures for different particle collection method and the collection positions.