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Lithium-ion battery cathode active material limn x fe 1-x po 4 The preparation method of /c

A positive electrode active material, lithium-ion battery technology, applied in the direction of battery electrodes, secondary batteries, chemical instruments and methods, etc., can solve the problem that lithium iron manganese phosphate is not a uniform single-phase crystal, and achieve uniformity consistent effect

Inactive Publication Date: 2016-08-10
SHANGHAI BYD
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  • Description
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Problems solved by technology

[0005] In order to solve the technical problem that lithium manganese iron phosphate is not a uniform single-phase crystal in the existing preparation method of lithium manganese iron phosphate, the present invention provides a method for preparing lithium manganese iron phosphate with uniform single-phase crystal

Method used

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  • Lithium-ion battery cathode active material limn <sub>x</sub> fe <sub>1-x</sub> po <sub>4</sub> The preparation method of /c
  • Lithium-ion battery cathode active material limn <sub>x</sub> fe <sub>1-x</sub> po <sub>4</sub> The preparation method of /c
  • Lithium-ion battery cathode active material limn <sub>x</sub> fe <sub>1-x</sub> po <sub>4</sub> The preparation method of /c

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preparation example Construction

[0023] The invention provides a lithium ion battery cathode active material LiMn x Fe 1-x PO 4 The preparation method of / C, the method may further comprise the steps:

[0024] S1, mixing soluble divalent manganese salt and soluble ferrous salt evenly to form a manganese-ferric salt mixture;

[0025] S2. Under the protection of inert gas, mix ferromanganese salt with complex precipitation agent, and prepare Mn by co-precipitation x Fe 1-x C 2 o 4 2H 2 O precursor;

[0026] S3, washing and drying the precursor to obtain precursor powder;

[0027] S4, under the protection of inert gas, the Mn x Fe 1-x C 2 o 4 2H 2 O precursor is mixed with soluble lithium salt and phosphate to obtain a precursor solution;

[0028] S5, reacting the precursor solution in an airtight container protected by an inert gas to obtain a reactant solution;

[0029] S6. After emulsifying and dispersing the carbon source into the reactant solution, dry it to obtain a mixture powder, sinter th...

Embodiment 1

[0053] 1L of 0.1mol / l concentration of ferrous sulfate and 1L of 0.1mol / l concentration of manganous sulfate solution were added dropwise to 1L of 0.2mol / l concentration of oxalic acid solution, while using ammonia to control the pH of the reaction solution to 7. Stir and react under circulating water at 40°C for 3 hours. After the reaction solution is left to age for 24 hours, filter, wash and dry to obtain light yellow Mn 0.5 Fe 0.5 C 2 o 4 2H 2 O Material A1.

[0054] 0.1mol of Mn 0.5 Fe 0.5 C 2 o 4 2H 2 O powder, 0.1mol lithium hydroxide, and 0.1mol phosphoric acid were added to 1L of deionized water, and the mixed solution was ball-milled in a ball mill for 1 hour, and then the solution after ball milling was transferred to a hydrothermal reaction kettle, under the protection of N2 at 180°C, After reacting for 16 hours under 1000rpm stirring, it was naturally cooled to room temperature, and the solution after the reaction was filtered, washed and dried 4 times to...

Embodiment 2

[0057] Add 1L of 0.4mol / l concentration of ferrous nitrate and 1L of 0.8mol / l concentration of manganous nitrate solution to 2L of 0.6mol / l concentration of sodium oxalate solution at the same time, and use sodium hydroxide to control the concentration of the reaction solution. The pH is 7.8, stirred and reacted for 4 hours under circulating water at 60°C, and the reacted solution was left to age for 48 hours, filtered, washed and dried to obtain light yellow Mn 0.67 Fe 0.33 C 2 o 4 2H 2 O material A2.

[0058] 0.5mol of Mn 0.67 Fe 0.33 C 2 o 4 2H 2 O powder and 0.5mol lithium dihydrogen phosphate were added to 1L of deionized water respectively, and the mixed solution was sand-milled in a sand mill for 2 hours, and the sand-milled solution was transferred to a hydrothermal reaction kettle. 1000rpm stirred and reacted for 24 hours, then naturally cooled to room temperature, and the solution after the reaction was filtered, washed and dried 4 times to obtain LiMn 0.67...

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Abstract

The invention provides a method for preparing LiMnxFe1‑xPO4 / C, a positive electrode active material for lithium ion batteries. The method includes the following steps: S1. Mix soluble divalent manganese salt and soluble ferrous salt to form a manganese iron salt mixture; S2. Mix the ferromanganese salt with the complex precipitant under the protection of inert gas, and co-precipitate to prepare MnxFe1‑xC2O4·2H2O; S3, wash and dry the precursor; S4, under the protection of inert gas, mix MnxFe1‑xC2O4·2H2O with soluble A precursor solution is obtained after mixing lithium salt and phosphate; S5, react the precursor solution in a closed container protected by inert gas to obtain a reactant solution; S6, add carbon to the reactant solution, dry it to obtain a mixture powder, and The mixture powder is sintered at high temperature and coated with carbon. Manganese and iron are evenly distributed in the material prepared by the method of the present invention, and no obvious iron-rich or manganese-rich areas appear.

Description

technical field [0001] The invention belongs to the field of lithium ion batteries, in particular to a lithium ion battery cathode active material LiMn x Fe 1-x PO 4 / C preparation method. Background technique [0002] At present, there are two reported preparation methods of lithium manganese iron phosphate: one is a high-temperature solid-phase method; the other is a traditional hydrothermal method. [0003] The method for preparing lithium manganese iron phosphate by the traditional high-temperature solid-phase method, such as the patent CN201110322643, uses lithium, manganese, iron, phosphate and a small amount of doping elements to be ball-milled, sand-milled or stirred and dispersed, and then pre-sintered at high temperature. Then add a carbon source for ball milling, sand milling or stirring, dispersing and mixing, and finally sintering at high temperature, and finally ball milling and crushing the sintered product to obtain a lithium iron phosphate material. The ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/58C01B25/45
CPCC01B25/45H01M4/5825H01M10/0525Y02E60/10
Inventor 陈靖华丁芳芳徐茶清肖峰
Owner SHANGHAI BYD
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