一阶FeCl_3-NiCl_2-GICs的制备与三元化评价

Preparation and Ternary Process Appraisal of Stage 1 FeCl_3-NiCl_2-GICs

采用熔盐法,以天然鳞片石墨为宿主,FeCl3与NiCl2的混合物为插层剂制备三元FeCl3-NiCl2-GICs.通过正交试验考察了石墨粒度、反应温度,保温时间及反应物配比等因素对产物阶结构及Ni元素分布的影响.提出了4个指标作为三元GICs阶结构完善程度及三元化进程的评价标准,它们分别为一阶相的体积分数V1、单个鳞片内Ni元素分布的均匀程度σ、试样中Ni元素的相对含量S和产物中Ni,Fe元素的物质的量之比与反应物中NiCl2,FeCl3即Ni,Fe元素的物质的量之比的比S′.确立了制备一阶FeCl3-NiCl2-GICs的最优工艺条件:石墨粒度为325目,保温时间为24 h,反应温度为450℃及石墨与氯化铁、氯化镍的配比为36∶9∶3.

Stage 1 FeCl3-NiCl2-GICs were synthesized in the molten salt method, using natural graphite flake as the host and a mixture of NiCl2 and FeCl3 as the guest. The effects of graphite granularity, the mole ratio of FeCl3 to NiCl2, the reaction temperature and reaction time on the stage structure, the Ni content and its distribution of the products were studied with four established criterions reflecting the ternary intercalation reaction process in the orthogonal experimental method. When the graphite granularity was 325 mesh, the reaction time was 24 h, the reaction temperature was 450 ℃ and the molar ratio of FeCl3 to NiCl2 was 9：3（the molar ratio of carbon to metal chlorides was 3：1 ）, the optimal stage 1 ternary FeCl3-NiCl2-GICs could be obtained.