Identification of Iron Carbides in Fe(−Na−S)/α-Al2O3 Fischer-Tropsch Synthesis Catalysts with X-ray Powder Diffractometry and Mössbauer Absorption Spectroscopy
Pasi P. Paalanen (Debye Institute)
Sophie H. van Vreeswijk (Debye Institute)
Iulian Dugulan (TU Delft - RID/TS/Instrumenten groep)
Bert M. Weckhuysen (Debye Institute)
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Abstract
In Fe-based Fischer-Tropsch Synthesis (FTS), the Fe carbides form under the carburizing H2 : CO reaction atmosphere providing the active phases for hydrocarbon synthesis. H2 reduced Fe(−Na−S)/α-Al2O3 catalyst materials, with and without Na−S promotion, were carburized under CO at 240–440 °C to form Fe carbides. X-ray Powder Diffractometry (XRPD) with Rietveld Quantitative Phase Analysis (R-QPA) and Mössbauer Absorption Spectroscopy (MAS) were used to identity and quantify the formed Fe carbide phases. The Fe carbides formed in order of increasing temperature are ϵ-Fe3C, η-Fe2C, χ-Fe5C2 and θ-Fe3C. θ-Fe7C3 and a distorted χ-Fe5C2 phase are formed at 25 bar CO (340 °C) from a Fe oxide precursor. Fe carbide formation was unaffected by Na−S addition, but it did increase Fe oxidation (≤290 °C) and preferred formation of χ-Fe5C2 over θ-Fe3C phase (≥390 °C). The results unify the often ambiguous Fe carbide identification and nomenclature and specify the role of Na−S in the carburization process.
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