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Preparation method of high-compaction-density lithium manganese iron phosphate/carbon composite positive electrode material

A technology of lithium iron manganese phosphate, positive electrode material, applied in nanotechnology, positive electrode, phosphorus compound and other directions for materials and surface science, can solve the problem of material compaction density not improving

Active Publication Date: 2021-07-06
天津斯科兰德科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The above published patents use different methods to synthesize lithium manganese phosphate or iron-doped lithium manganese phosphate material, but the compaction density of the material is not improved

Method used

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  • Preparation method of high-compaction-density lithium manganese iron phosphate/carbon composite positive electrode material
  • Preparation method of high-compaction-density lithium manganese iron phosphate/carbon composite positive electrode material
  • Preparation method of high-compaction-density lithium manganese iron phosphate/carbon composite positive electrode material

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preparation example Construction

[0035] Concrete preparation method comprises the following steps:

[0036] 1) Dilute phosphoric acid to a mass concentration of 2-55% for later use, add manganese source, iron source, dispersant and deionized water in a sealable container, and pass protective gas into the container;

[0037] 2) Slowly add the diluted phosphoric acid solution into a sealed container to produce ferromanganous phosphate precipitation, age for 10-20 days, and adjust the pH value at any time to stabilize at 2.0-5.0, so that it can nucleate uniformly;

[0038] 3) Wash the formed precipitate with 5-50 times the mass of deionized water for 3-5 times, then dry it in vacuum at 60-80°C, and then sinter at high temperature in a protective gas atmosphere for the first time to form spherical particles of 1-10 μm A;

[0039] 4) Take lithium hydroxide monohydrate LiOH·H 2 O is prepared into a solution with a mass concentration of 1 to 15%, adding spherical particles A to it, spraying and drying, and sinteri...

Embodiment 1

[0049] 1) Weigh 28.7ml of 85% phosphoric acid and slowly add 200ml of deionized water to dilute and prepare a solution for later use. Add 45.30g of manganese sulfate MnSO in a sealed container 4 , 55.61g ferrous sulfate heptahydrate FeSO 4 ·7H 2 0, 4g Polyethylene Glycol 400 and 100ml deionized water, pass into nitrogen protective gas in this container.

[0050] 2) Slowly add diluted phosphoric acid into a sealed container to produce ferromanganous phosphate precipitation, age for 15 days, and adjust the pH value to 4.0 at any time to make it evenly nucleate.

[0051] 3) The formed precipitate was washed 4 times with 10 ml of deionized water, and then dried under vacuum at 60°C. Then sinter for the first time at a high temperature of 750° C. for 5 hours in a nitrogen protective gas atmosphere to form spherical particles A of 1-10 μm.

[0052] 4) Take 20.98g lithium hydroxide monohydrate LiOH·H 2 O is prepared into a solution with a mass concentration of 10%, adding spheric...

Embodiment 2

[0055] 1) Weigh 28.7ml of 85% phosphoric acid and slowly add 200ml of deionized water to dilute and prepare a solution for later use. Add 37.77g of manganese dichloride MnCl in a sealed container 2 , 25.35g ferrous chloride FeCl 2 , 4g Polyethylene Glycol 400 and 100ml deionized water, pass into nitrogen protection gas in this container.

[0056] 2) Slowly add diluted phosphoric acid into a sealed container to produce ferromanganous phosphate precipitation, age for 12 days, and adjust the pH value to 4.0 at any time to make it evenly nucleate.

[0057] 3) The formed precipitate was washed 4 times with 15 ml of deionized water, and then dried under vacuum at 70°C. Then sinter for the first time at a high temperature of 720° C. for 8 hours in a nitrogen protective gas atmosphere to form spherical particles A of 1-10 μm.

[0058] 4) Take 20.98g lithium hydroxide monohydrate LiOH·H 2 O is prepared into a solution with a mass concentration of 10%, adding spherical particles A to...

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Abstract

The invention discloses a preparation method of a high-compaction-density lithium manganese iron phosphate / carbon composite positive electrode material. The chemical general formula of the material is LiMnxFeyPO4 / C, wherein x is more than or equal to 0.5 and less than or equal to 0.9, and x + y is equal to 1. The preparation method comprises the following steps: diluting phosphoric acid for later use, adding a manganese source, an iron source, a dispersing agent and deionized water into a sealable container, and introducing shielding gas; adding diluted phosphoric acid into the sealed container, aging until the pH value is 2.0-5.0, and uniformly nucleating; cleaning the formed precipitate, drying in vacuum, and sintering for the first time at high temperature to form spherical particles A; preparing a solution from lithium hydroxide monohydrate, adding the spherical particles A into the solution, performing spray drying, and performing high-temperature secondary sintering to obtain spherical particles B; and preparing a glucose solution, adding the spherical particles B into the glucose solution, performing spray drying, and performing high-temperature third sintering to obtain the nano spherical lithium manganese iron phosphate / carbon composite material. The electrochemical performance and the compaction density of the material are greatly improved.

Description

technical field [0001] The invention belongs to the technical field of energy storage materials, and in particular relates to a preparation method of a high compacted density lithium manganese iron phosphate / carbon composite cathode material. Background technique [0002] The application of lithium-ion batteries (LIBs) in hybrid and electric vehicles has attracted considerable academic and industrial research interest. Since the pioneering work of Goodenough's group in 1997, olivine-structured polyanionic phosphate materials (LiMPO 4 , M = Fe, Mn, Co, and Ni) have been widely studied as cathode materials due to their high theoretical capacity, thermal stability, and environmental friendliness. Based on safety requirements, LiFePO 4 (LFP) has been successfully used in LIBs as an alternative LiMnPO 4 (LMP) provides the same theoretical specific capacity (170mAh g -1 ), and with Fe 2+ / Fe 3+ Compared to Mn 2+ / Mn 3+ The redox potential of LMP is higher, thus making the ...

Claims

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Application Information

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IPC IPC(8): C01B25/45C01B32/00H01M4/58H01M4/62H01M10/0525B82Y30/00
CPCC01B25/45C01B32/00H01M4/5825H01M4/625H01M10/0525B82Y30/00H01M2004/021H01M2004/028C01P2004/32C01P2004/80C01P2006/40C01P2006/11Y02E60/10
Inventor 李积刚
Owner 天津斯科兰德科技有限公司
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