熔盐法合成三元FeCl3-NiCl2-石墨层间化合物的研究

熔盐法合成三元FeCl3-NiCl2-石墨层间化合物的研究

  • 摘要: 采用熔盐法,以天然鳞片石墨为宿主,NiCl2与FeCl3的混合物为插层剂合成三元FeCl3-NiCl2-GIC。考察了石墨与氯化物的摩尔比、NiCl2与FeCl3的摩尔比、反应温度和反应时间等工艺因素对产物阶结构和产物中Ni与Fe原子比的影响,探讨了NiCl2与FeCl3在石墨层间的插层过程。研究结果表明,改变反应体系中石墨与氯化物的摩尔比、NiCl2与FeCl3的摩尔比、反应温度和恒温时间,可以得到阶结构和Ni/Fe原子比不同的FeCl3-NiCl2-GIC,产物中的Ni/Fe原子比随反应体系中NiCl2与FeCl3的摩尔比的增大、反应温度的提高而增加。当石墨/氯化物的摩尔比为3∶1,NiCl2/FeCl3的摩尔比为3∶7,反应温度为400℃,反应时间为72h时,所得产物为一阶FeCl3-NiCl2-GIC。反应过程中存在FeCl3先插入石墨层间,然后NiCl2逐渐替换FeCl3的插层反应机制。

     

    Abstract: Abstract: Ternary FeCl3-NiCl2-GICs were synthesized by the molten salt method, with natural graphite flake used as host and a mixture of NiCl2 and FeCl3 as guest. The effect of molar ratio of carbon to metal chlorides, molar ratio of NiCl2 to FeCl3, reaction temperature and reaction time on the stage structure and the Ni/Fe molar ratio of the products, as well as the intercalation reaction process of NiCl2 and FeCl3 between graphite layers were studied. The results show that ternary FeCl3-NiCl2-GICs with different stage structure and molar ratio of Ni to Fe could be obtained through changing the molar ratio of carbon to metal chlorides, molar ratio of NiCl2 to FeCl3, reaction temperature and reaction time. The molar ratio of Ni to Fe of the products increased with increasing molar ratio of NiCl2 to FeCl3 and intercalation reaction temperature. When the molar ratio of carbon to metal chlorides is 3:1 and the molar ratio of NiCl2 to FeCl3 is 3:7, stage one FeCl3-NiCl2-GIC was obtained at 400℃ in three days. The intercalation reaction mechanism may be considered as FeCl3 being gradually replaced by NiCl2.

     

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