Iron as Recyclable Metal Fuel: Unraveling Oxidation Behavior and Cyclization Effects Through Thermogravimetric Analysis, Wide‐Angle X‐ray Scattering and Mössbauer Spectroscopy

The carbon-free chemical storage and release of renewable energy is an important task to drastically reduce CO2 emissions. The high specific energy density of iron and its recyclability makes it a promising storage material. Energy release by oxidation with air can be realized by the combustion of micron-sized iron powders in retro-fitted coal fired power plants and in fixed-bed reactors under milder conditions. An experimental parameter study of iron powder oxidation with air was conducted based on thermogravimetric analysis in combination with wide-angle X-ray scattering and Mössbauer spectroscopy. In agreement with literature the oxidation was found to consist of a very fast initial oxidation of the outer particle layer followed by much slower oxidation due to diffusion of iron ions through the Fe2O3/Fe3O4 layer being the rate-limiting step. Scanning electron microscopy analysis of the iron particle before and after oxidation reveal a strong particle morphology transformation. This impact on the reaction was studied by cyclization experiments. Up to 10 oxidation-reduction cycles show that both, oxidation and reduction rates, increase strongly with cycling due to increased porosity.