In situ 57Mössbauer spectroscopy has been used to study the process of reduction and Fischer-Tropsch reactions on FeCl 3 intercalated in graphite layers. It is found that on flowing H 2 on graphite intercalated by FeCl 3 at 400° C, FeCl 3 converts to FeCl 2 and partly to small particles of α-Fe. The Mössbauer spectra of the reduced sample are superposition of a sextuplet and two quadrupole doublets indicative of metallic iron and two species of FeCl 2. However, at room temperature and at 400° C for a short period of reduction the magnetic hyperfine splittings ( ca. 295 kOe and 262 kOe respectively) are smaller than the corresponding parameters for bulk metallic iron. The differences have been attributed to the interaction between the monolayers of iron atoms and the carbon nets of the graphite support. When the reduction was carried out for a longer period, α-Fe was formed. When a sample reduced for a short period of time is heated at 400°C in the presence of the synthesis gas, part of the iron particles sinter, and α-iron is observed. On heating the above sample once again at 400°C in the presence of the synthesis gas, the remaining small particles of iron are totally converted to the bulk phase (α-Fe). Experimental observations indicate that α-Fe and FeCl 2 are present on the surface as well as inbetween the intercalated graphite layers.
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