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a limn x fe 1‑x po 4 Positive electrode active material and preparation method thereof

A cathode active material, mnxfe1-xco3 technology, applied in the field of LiMnxFe1-xPO4 cathode active material and its preparation, can solve the problems of large particle size, low temperature performance and low discharge efficiency at high rate, and achieve stable material performance and short time consumption , The effect of material particle uniformity

Active Publication Date: 2017-10-13
BYD CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The present invention is in order to solve the LiMn prepared by prior art x Fe 1-x PO 4 Large particle size, low temperature performance and low high rate discharge efficiency, LiMn prepared at the same time x Fe 1-x PO 4 It is not a shortcoming of a uniform single-phase lithium manganese iron phosphate material. It provides a single-phase LiMn with small particle size, low temperature performance and high rate discharge efficiency. x Fe 1-x PO 4 and its preparation method

Method used

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  • a limn <sub>x</sub> fe <sub>1‑x</sub> po <sub>4</sub> Positive electrode active material and preparation method thereof
  • a limn <sub>x</sub> fe <sub>1‑x</sub> po <sub>4</sub> Positive electrode active material and preparation method thereof
  • a limn <sub>x</sub> fe <sub>1‑x</sub> po <sub>4</sub> Positive electrode active material and preparation method thereof

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preparation example Construction

[0024] The invention provides a LiMn x Fe 1-x PO 4 A method for preparing a positive electrode active material, the method comprising the steps of:

[0025] S1. Mix soluble divalent manganese salt and soluble ferrous salt to form a mixed solution; then under the protection of an inert gas, mix the mixed solution and carbonate to form a reaction solution for reaction, and control the pH of the reaction solution to 3-5, get Mn x Fe 1- x CO 3 Precursor;

[0026] S2, under an inert atmosphere, the Mn prepared in step S1 x Fe 1-x CO 3 The precursor is mixed with lithium source, phosphorus source and water, dried, and then calcined to obtain LiMn x Fe 1-x PO 4 ;

[0027] Among them, 0

[0028] LiMn of the present invention x Fe 1-x PO 4 In the preparation method of the positive electrode active material, soluble divalent iron salt and soluble divalent manganese salt are used, the valence state of iron and manganese is consistent, and the ratio of iron and mangane...

Embodiment 1

[0049] 1. Preparation of positive electrode active material:

[0050] 97.3gFeSO 4 .7H 2 O was dissolved in deionized water by mechanical stirring to make 1L 0.35molL -1 FeSO 4 .7H 2 O solution, followed by 109.9g MnSO 4 .H 2 O dissolved in 0.35molL -1 FeSO 4 .7H 2 0.65molL in O solution -1 MnSO 4 .H 2 O solution, 158.12g NH 4 HCO 3 Dissolve in deionized water by mechanical stirring to make 1L 2molL -1 NH 4 HCO 3 solution, through a metering pump at 25mL min -1 rate while FeSO 4 .7H 2 O, MnSO 4 .H 2 The mixed solution formed by O and NH 4 HCO 3 The solution was poured into the emulsifier for reaction, and acetic acid was added to adjust the pH to 3, and the emulsification was carried out when the solution was just in contact with the reaction, and the reaction product obtained after emulsification for 1 hour was washed with a centrifuge, and the washed product was dried with nitrogen gas After obtaining nanoscale pure phase Mn 0.65 Fe 0.35 CO 3 .

[005...

Embodiment 2

[0059] 1. Preparation of positive electrode active material:

[0060] 98.955gMnCl 2 .4H 2 O was dissolved in deionized water by mechanical stirring to make 1L 0.5molL -1 FeCl 2 solution, followed by 63.375g FeCl 2 Dissolved in 0.5molL -1 MnCl 2 .4H 2 0.5molL in O solution -1 MnCl 2 .4H 2 O solution, and in this mixed solution, add 58g ascorbic acid, adjust pH to be 5. 202g NaCO 3 Dissolve in deionized water by mechanical stirring to make 1L 2molL -1 NaCO 3 solution, through a metering pump at 25mL min -1 Simultaneously flow into the emulsifier at the same rate to react, and emulsify when the solution is just in contact with the reaction, the reaction product obtained after emulsification for 1 hour is washed with a centrifuge, and the washed product is dried with nitrogen to obtain nano-scale pure phase Mn 0.5 Fe 0.5 CO 3 .

[0061] Weigh 115.30 g of 85% H 3 PO 4 , 24.42 gLiOH to make a 1mol / L solution, slowly drain the prepared phosphoric acid solution into...

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Abstract

The invention provides a preparation method of a LiMnxFe1-xPO4 positive electrode active material. The method comprises the following steps that soluble divalent manganese salt and soluble divalent ferric salt are blended to form a mixed solution, the mixed solution and carbonate are mixed and undergo a reaction to produce a MnxFe1-xCO3 precursor, and LiMnxFe1-xPO4 is prepared from the MnxFe1-xCO3 precursor. The invention also provides the LiMnxFe1-xPO4 positive electrode active material obtained by the preparation method. The LiMnxFe1-xPO4 positive electrode active material has the advantages of uniform particle size distribution, perfect morphology, no agglomeration, small particle size and material electroconductivity improvement. A cell prepared from the LiMnxFe1-xPO4 positive electrode active material has excellent rate discharge performance, especially has high-rate discharge performance, has a high cell charging-discharging capacity, stable cell charging-discharging performances and good cycle performances, lays the foundation in excellent positive electrode active material development and is conducive to material application and cell development.

Description

technical field [0001] The invention belongs to the field of lithium ion batteries, in particular to a LiMn x Fe 1-x PO 4 Positive electrode active material and preparation method thereof. Background technique [0002] As a high-energy chemical power source, lithium-ion batteries have been widely used in mobile communications, notebook computers, video cameras, cameras, portable instruments and other fields. . [0003] Lithium-ion battery cathode material is a hot and difficult point in the existing technology research, commonly used such as LiFePO 4 , has good electrochemical performance, very stable charging and discharging platform, stable structure during charging and discharging, and has the advantages of non-toxic, non-polluting, good safety performance, can be used in high temperature environments, and a wide range of raw materials. It is currently the battery industry Competitively developed materials. But LiFePO 4 relative to Li + The electrode potential of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/58H01M4/1397
CPCH01M4/136H01M4/1397H01M4/5825H01M2004/028Y02E60/10
Inventor 游军飞徐茶清肖峰
Owner BYD CO LTD
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