Transition metals supported on carbons play an important role in catalysis and energy storage. By pyrolysis of metal alginate, highly active catalysts for the Fischer-Tropsch synthesis (FTS) can be produced. However, the evolution of the carbon (alginate) and transition metal (Fe³⁺) during pyrolysis remains largely unknown and was herein corroborated with several advanced in situ techniques. Initially, Fe³⁺ was reduced to Fe²⁺, while bound to alginate. FeO nucleated above 300 °C, destabilizing the alginate functional groups. Increasing temperatures improved carbonization of the carbon support, which facilitated reduction of FeO to α-Fe at 630 °C. Catalysts were produced by pyrolysis between 400 and 700 °C, where the highest FTS activity (612 µmol_CO g_Fe⁻¹ s⁻¹) was achieved for the sample pyrolyzed at low temperature. Lower metal loading, due to less decomposition of alginate, moderated sintering and yielded larger catalytic surface areas. The results provide valuable knowledge for rational design of metal-alginate-based materials.