Fluorinated ferric sulfate salt compound as well as preparation method and application thereof
A technology of fluorinated sulfuric acid and compound, applied in the field of materials, can solve the problems of unsatisfactory structural stability of fluorinated sulfate, difficult mass production, and limited application of secondary lithium batteries, etc.
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[0079] The preparation method of described fluorinated ferric sulfate compound, comprises the steps:
[0080] 1), according to the molar ratio of each element in the general formula, weigh Li source, Fe source, fluorine source, SO 4 2- source and M source, mixed and ground to obtain precursor powder;
[0081] 2) Hot pressing and sintering the precursor powder to obtain the fluorinated ferric sulfate compound. During the sintering process, a mechanical pressure greater than atmospheric pressure is applied to the precursor powder, preferably greater than or equal to 0.5 MPa.
[0082] Optionally, before the hot pressing sintering of the precursor powder, it is pre-fired in an inert atmosphere or an inert atmosphere containing a reducing gas for 0.5-10 hours, and the pre-fire temperature is 100-300°C. The function of pre-firing is mainly to remove moisture from the precursor powder to dry it. The precursor powder is placed in an inert atmosphere or an inert atmosphere containin...
Embodiment 1
[0152] Monoclinic crystal system with mixed cation occupancy (Li 0.5 Fe 0.5 ) 2 SO 4 f
[0153] (Li 0.5 Fe 0.5 ) 2 SO 4 F is prepared by the following steps: First, weigh LiF and FeSO in a molar ratio of 1:1 4 ·7H 2 O (or FeSO 4 ·H 2 (2), adopting Union Process 01-HD type high-energy ball mill ball milling to obtain D50 after 5 hours is the precursor powder of 30nm, wherein ball milling medium particle diameter 0.1mm-10mm, rotating speed is 2000 rev / min; This precursor powder is in high-purity Pre-fired under the protection of Ar gas for 5 hours, the pre-fired temperature is 200°C (the pre-fired temperature rise rate is 1 hour to increase the temperature of the precursor powder from room temperature to 200°C), and then cool down to room temperature for 10 hours; grind and pre-fire The final precursor powder was hot-pressed and sintered at a constant temperature of 380° C. (the heating rate was 2 hours from room temperature to 380° C.) for 0.25 hours, and the hot-pre...
Embodiment 2
[0168] Monoclinic crystal system with mixed cation occupancy (Li 0.6 Fe 0.4 ) 2 SO 4 f
[0169] (Li 0.6 Fe 0.4 ) 2 SO 4F is prepared by the following steps. First, weigh LiF and FeSO according to the molar ratio of 1.2:0.8 4 ·7H 2 O (or FeSO 4 ·H 2 (O), then adopt the same method as in Example 1 to obtain the monoclinic (Li 0.6 Fe 0.4 ) 2 SO 4 F cathode material.
[0170] The crystal structure, discharge capacity and first-week discharge rate were tested by XRD and constant current charge-discharge instrument. The XRD measured graph and first-week charge-discharge curve of the compound sample were shown Figure 4-2 and 5-2 As shown, the average particle size, discharge capacity, and first-week efficiency data are shown in Table 4.
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