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Preparation method of lithium ferrite

A technology of lithium ferrite and iron source, applied in chemical instruments and methods, electrode manufacturing, iron compounds, etc., can solve the problem of high impurity content in products

Active Publication Date: 2020-12-22
SHENZHEN DYNANONIC INNOVAZONE NEW ENERGY TECH CO LTD +2
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a preparation method of lithium ferrite, aiming to solve the technical problem of high impurity content of the product existing in the preparation method of lithium ferrite

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  • Preparation method of lithium ferrite

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preparation example Construction

[0035] The embodiment of the present invention provides a preparation method of lithium ferrite, which comprises the following steps:

[0036] S1. Mixing iron source, lithium source and organic acid in a solvent to obtain a mixed solution;

[0037] S2, the mixed solution is heated to obtain a precursor solution;

[0038] S3. The precursor solution is dried and sintered to obtain lithium ferrite.

[0039] In the preparation method of lithium ferrite provided in the embodiment of the present invention, on the one hand, the iron source, lithium source and organic acid are mixed in an aqueous solvent by using a solvent method to obtain iron hydroxide colloid with a smaller particle size. In this process, since the lithium source is an alkaline compound, it is easy to make the ferric hydroxide colloid in the reaction system become ferric hydroxide precipitate, so an organic acid needs to be added to reduce the generation of ferric hydroxide precipitate. At the same time, the organi...

Embodiment 1

[0056] This embodiment provides a kind of preparation method of lithium ferrite, the steps are as follows:

[0057] Fe(NO 3 ) 3 9H 2 O 0.10mol was dissolved in a mixed solvent of 100mL distilled water and 20mL ethanol, and stirred in an ice-water bath. Take 3mol / L LiCH 3 COO and 1mol / L Li 2 CO 3 The solution was slowly dropped into the above solution, so that the LiCH 3 The amount of substance added by COO is 0.20mol; Li 2 CO 3The amount of the substance added is 0.20 mol, and oxalic acid is added during the titration process to ensure that the pH is less than or equal to 3.7. Then put it into a reaction kettle, and carry out a solvothermal reaction at 150° C. After the reaction is completed, the solution is spray-dried to obtain a precursor material. The precursor material was incubated in air at 500°C for 10 hours, and then held in an argon atmosphere at 900°C for 3 hours to obtain Li 5 FeO 4 . The purity of the obtained lithium ferrite was detected, and the resu...

Embodiment 2

[0059] This embodiment provides a kind of preparation method of lithium ferrite, the steps are as follows:

[0060] Fe(NO 3 ) 3 9H 2 O 0.10mol was dissolved in 120mL distilled water, stirred in an ice-water bath, and 2mol / L LiCH 3 COO and 2mol / L Li 2 CO 3 The solution was slowly dropped into the above solution, LiCH 3 The amount of substance added by COO is 0.3mol; Li 2 CO 3 The amount of the substance added is 0.15 mol, and acetic acid is added during the titration process to ensure that the pH is ≤ 3.7. Then put it into a reaction kettle, and perform a solvothermal reaction at 150°C, and the solution after the reaction is spray-dried to obtain a precursor material. The precursor material was incubated in air at 600°C for 6 hours, and then held at 850°C in an argon atmosphere for 6 hours to obtain Li 5 FeO 4 , its XRD data such as figure 1 As shown, its microstructure is as Figure 4 shown. pass figure 1 As can be seen, figure 1 Two characteristic peaks of the ...

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Abstract

The invention belongs to the technical field of lithium supplementing materials of lithium ion batteries, and particularly relates to a preparation method of lithium ferrite. By adopting a solvent method, an iron source, a lithium source and organic acid are mixed in a water-containing solvent to obtain ferric hydroxide colloid with smaller particle size. Meanwhile, the organic acid reacts with alithium source to generate a lithium salt, and the lithium salt and the ferric hydroxide colloid can be attached to the surface of the ferric hydroxide colloid after being heated to form a precursor solution with higher activity. And after the obtained precursor solution is dried, lithium ferrite with relatively high purity can be obtained only by once sintering, so the problems of repeated sintering, insufficient sintering reaction, long sintering time and high impurity content of a conventional solid-phase method are solved.

Description

technical field [0001] The invention belongs to the technical field of lithium supplementary materials for lithium ion batteries, and in particular relates to a preparation method of lithium ferrite. Background technique [0002] With the rapid development of energy storage technology, the use of portable digital devices and vehicle-mounted power supplies is increasing, and people have higher and higher requirements for the energy density of batteries. It is imperative to develop secondary batteries with large capacity, long life and high safety. Row. [0003] During the first charge and discharge process of lithium-ion batteries, an SEI film will be formed at the interface of the negative electrode material. Studies have shown that the main components of SEI are LiF, Li 2 CO 3 , R-COOLi, R-CH 2 Lithium salt materials such as OLi. The formation of SEI is an irreversible process, the Li used to form SEI + It can no longer be embedded in the cathode material during discha...

Claims

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Application Information

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IPC IPC(8): H01M4/04H01M4/525H01M10/0525C01G49/00
CPCH01M4/0471H01M4/525H01M10/0525C01G49/0027Y02E60/10
Inventor 赵中可万远鑫孔令涌任望保钟泽钦周永辉朱成奔张於财
Owner SHENZHEN DYNANONIC INNOVAZONE NEW ENERGY TECH CO LTD
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