| Transition metal Chloride-graphite intercalation compounds (GICs) are a kind of material with special structure and properties. They become the focus among the research of GICs in the latest 20 years because of good physical and chemical properties, such as high conductivity and catalysis, and good structural and capability stability, including which can be bulkily synthesized. However, it is very scarce the research on transition metal chloride-GICs to be reduced to magnetism and in-situ catalysis transition metal-GICs at home and abroad. As a new method of synthesis of transition metal-GICs, it shall be greatly promoting research process on GICs. So based on the experiment of synthesis of FeCl3-NiCl2-GICs, the possibility of synthesis of transition metals-GICs,which reduced by H2, and the FeCl3-NiCl2-GICs reduction conditions in flowing H2 was basically discussed in our present work.FeCb-NiCb-GICs had been synthesized through molten salts method. The natural graphite powder was used as host material and the mixture of NiCl2 and FeCl3 was as intercalant .The paper discussed the influence of reaction conditions such as temperature and time as well as the chlorides molar ratios on the products stage structure and its Ni/Fe molar ratios. The intercalation process was also discussed. The results showed that with the change of molar ratios among graphite, FeCl3 and NiCl2, and the change of reaction time and temperature, FeCl3-NiCl2-GICs, with different stages and Fe/Ni ratios, could be obtained. The products Ni/Fe molar ratio increased with the increasing of NiCl2/FeCl3 molar ratio and reaction temperature. Under the conditions of C/chlorides=3:l, NiCl2/FeCl3=3:7, 400, 72h, the product was approximately a pure stage one FeCl3-NiCl2-GIC. During the reaction process, NiCl2 partially took the place of FeCl3 which was intercalated preferentially.From the characteristic of synthesis of FeCl3-NiCl2-GICs and the result analysis, it could be concluded that during the process of FeCl3 and NiCl2 being intercalated into the graphite, the reaction process may be divided into several steps as follows: evolution of transportable species; absorption of the intercalate onto the surface (or edge) of the host graphite; insertion of the intercalate into the gallery of the host ; diffusion occurred at the interface between the initial stage and pristine graphite. The dynamic of FeCl3 and NiCl2 intercalation into graphite arose from temperate and C12 pressure in the system, and the two mental chlorides exchange and diffusion among graphite layers controlled the reaction rate .The intercalants remained as islands in graphite layers. The formationiiand transform of stages resulted from the islands diffusion and dislocations remove.After synthesis of FeCla-NiCb-GICs, which were reduced by Fk in hope of getting magnetic and catalyst Fe-Ni-GIC, we basically discussed the influence of flow rate of H2, the means of increasing reaction temperature and reduction time on the stage structure and C/(Fe+Ni) molar ratio. The reduction condition was basically concluded. The results showed that lowering the starting temperature, then gradually upgrading temperature for several steps, FeCU-NiCh-GIC can be partially reduced to Fe-Ni-GICs in flowing Fk. The Cl/(Fe+Ni) molar ratio of the reduction product became smaller with reduction temperature increase and reduction time prolong. The key reason of high proportion Cl in the reduction products was that Cl atoms were combined with graphite electrons to form firm chemical bonds. Another important reason was that H2 pressure in the system was too small.
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