Development of noble metal free cathode catalysts in fuel cells would be a significant step towards making fuel cell technology commercially applicable. Generally, fuel cells use platinum as both the anode and the cathode catalyst. For the oxidation reaction this is not problematic because very little Platinum is needed. For the reduction reaction, however, much more platinum is needed to make the fuel cell efficient and can therefore be very expensive. As an alternative cathode catalyst, this project explored metalloporphyrin like materials enriched with iron. Ordered mesoporous Fe-N/C materials were synthesized utilizing a carbon solution impregnation technique of Ia3d cubic silica followed by polymerization and pyrolysis. The hope is that these materials will rival the catalytic activity of platinum to be potentially used as a cheaper alternative. The synthesized materials were structurally characterized using small angle X-ray spectroscopy (SAXS), nitrogen physisorption (BET) and scanning electron microscopy (SEM) measurement techniques and tested for their catalytic activity in a polymer electrolyte fuel cell (PEMFC) using cyclic voltammetry. It was found that the precursors had a significant effect on the final structure and activity and that the addition of iron to the precursor significantly increased the activity for the four-electron oxidation-reduction reaction that occurs in a fuel cell.