Laser ablation was used to deposit nanoparticles of Fe on Al2O3 substrates which in turn were prepared by laser ablation onto Cu grids used in transmission electron microscopes. The Fe particles were covered by a thin amorphous carbon layer, in order to protect them from ambient oxidation as they were transferred to the TEM. Depth profiles of their chemical composition were preformed using Auger electron spectroscopy, in order to verify that the Fe particles were not oxidized. Using reported values of Electron Attenuation Length (λEAL) of Auger electrons corresponding to the C KLL transition, the carbon layer was determined to be less than 4 nm. Al2O3 deposits on the Cu grids show a polycrystalline structure dominated by δ‐phase, following measured interplanar distances. At room temperature, Fe particles show a faceted crystalline structure of approximately 10 nm in diameter. These particles were studied by Electron Energy Loss Spectroscopy (EELS). High resolution images show a lattice with an interplanar spacing of 0.2 nm which may correspond to the set (110) planes of Fe.