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Carbon spheres (CSs) synthesised by the hydrothermal approach were explored as a model support material for a bimetallic Fe–Co Fischer–Tropsch (FT) catalyst. The CSs were characterised by N2 adsorption–desorption, thermogravimetric analysis, FTIR spectroscopy and powder XRD. If annealed at 900 °C for 4 h, the CSs exhibited an improved surface area, thermal stability and crystallinity. A series of Fe–Co bimetallic FT catalysts supported on the annealed CSs were prepared by co‐precipitation. A variety of Fe‐to‐Co ratios were used with the total metal loadings maintained at 10 %. Catalyst reducibility studies were performed by H2 temperature‐programmed reduction and in situ powder XRD. Catalysts with a Fe/Co ratio of 5:5 (w/w) showed Co–Fe alloy formation upon reduction at >450 °C. Interestingly, the presence of this alloy did not correlate with high C5+ selectivities during FT synthesis; rather the Co‐rich/Fe‐poor catalyst gave the best selectivity. The CSs allowed the metal–metal interactions in the bimetallic systems to be monitored because of the weak interaction of the metals with the support.

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