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Method for preparing lithium manganese battery material lithium manganese phosphate/carbon by sol-gel

A lithium-ion battery, lithium manganese phosphate technology, applied in the direction of battery electrodes, circuits, electrical components, etc., can solve the problem of low purity of synthetic products, and achieve the effect of excellent electrochemical performance, uniform distribution, and high energy density

Inactive Publication Date: 2011-12-14
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the high-temperature solid-state reaction method is the most widely used. The domestic Wang Zhixing research group has conducted research on this for many years. The typical synthesis process is LiMnPO according to the composition. 4 The stoichiometric ratio of Li 2 CO 3 , MnCO 3 , NH 4 h 2 PO 4 , and mixed with an appropriate amount of carbon black ball mill, and then calcined in an inert atmosphere to obtain the product, but this method has the problem of low purity of the synthetic product

Method used

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  • Method for preparing lithium manganese battery material lithium manganese phosphate/carbon by sol-gel
  • Method for preparing lithium manganese battery material lithium manganese phosphate/carbon by sol-gel
  • Method for preparing lithium manganese battery material lithium manganese phosphate/carbon by sol-gel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Manganese citrate preparation:

[0025] Using manganese chloride and citric acid as raw materials, dissolve 9.9g of manganese chloride and 21g of citric acid in deionized water, adjust the pH value of the solution to 2.7 with ammonia water, and magnetically stir in a 60°C water bath. After stirring for about 30 minutes, a white precipitate appeared, and the reaction was continued for 5 hours until the solution was completely precipitated, treated with ultrasonic waves for 30 minutes, and filtered with suction to obtain manganese citrate compound.

[0026] 1) Precursor preparation: 0.78g Li 2 CO 3 , 5.26gMn(Hct) 2 , 2.3gH 3 PO 4 , 4.2gH(ct)2(Li:Mn:P:complexing agent=1.025:1:1:1) was dissolved in 100ml deionized water, stirred for 10 minutes, and the test pH value was 3.2, and the sol was obtained by magnetic stirring for a period of time solution, after the sol solution is clarified, place it in a 60°C water bath and evaporate to dryness until a xerogel is obtained;...

Embodiment 2

[0036] 1) Precursor preparation: 0.78g Li 2 CO 3 , 5.26gMn(Hct) 2 , 2.3gH 3 PO 4 , 4.2gH(ct)2(Li:Mn:P:complexing agent=1.025:1:1:1) was dissolved in 100ml deionized water, stirred for 10 minutes, and the test pH value was 3.2, and the sol was obtained by magnetic stirring for a period of time solution, after the sol solution is clarified, place it in a 60°C water bath and evaporate to dryness until a xerogel is obtained;

[0037] 2) Drying treatment: dry the obtained xerogel at 120°C to obtain a dry solid, take it out and grind it to obtain a precursor powder;

[0038] 3) roasting treatment: take a certain amount of the pulverized mixture in the above-mentioned process and put it in the ceramic ark. 2 (where H 2 The volume fraction is 10%), adopting the method of temperature programming, firstly, the mixture is heated to 350°C at a rate of 2°C / min and kept for 5h, then heated to 600°C at a rate of 5°C / min and kept for 3h, and then cooled naturally in the furnace To room...

Embodiment 3

[0041] 1) Precursor preparation: 0.78g Li 2 CO 3 , 5.26gMn(Hct) 2 , 2.3gH 3 PO 4 , 4.2gH(ct)2(Li:Mn:P:complexing agent=1.025:1:1:1) was dissolved in 100ml deionized water, stirred for 10 minutes, and the test pH value was 3.2, and the sol was obtained by magnetic stirring for a period of time solution, after the sol solution is clarified, place it in a 60°C water bath and evaporate to dryness until a xerogel is obtained;

[0042] 2) Drying treatment: dry the obtained xerogel at 120°C to obtain a dry solid, take it out and grind it to obtain a precursor powder;

[0043] 3) roasting treatment: take a certain amount of the pulverized mixture in the above-mentioned process and put it in the ceramic ark. 2 (where H 2 The volume fraction is 10%), using a temperature program method, firstly the mixture is heated to 350°C at a rate of 2°C / min and kept for 5h, then heated to 500°C at a rate of 5°C / min and kept for 3h, and then cooled naturally in the furnace To room temperature,...

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Abstract

The invention discloses a method for preparing lithium manganese phosphate lithium / carbon as a lithium ion battery material by using sol-gel, belonging to the technical field of new energy materials. In the preparation method, the lithium source compound, the manganese source compound, the phosphorus source compound and the complexing agent compound are dissolved or dispersed in a solvent in a molar ratio of 1.025:1:1:0-2 to obtain a mixed material. Concentrated nitric acid or Concentrated ammonia water is used to adjust the pH value of the solution to 0.5-3.7 to obtain a sol solution. The sol solution is evaporated to dryness in a water bath to obtain dry gel, which is then dried and calcined to obtain carbon-coated lithium manganese phosphate with a particle size of 50-150 nm. The material synthesized by the method has a nanoscale size and is evenly dispersed, and the lithium manganese phosphate matrix is ​​coated with a carbon material, which effectively prevents the agglomeration of the particles and improves the electronic conductivity of the particles. Electrochemical tests show that the electrode has an obvious discharge platform at about 4V, high discharge capacity, and good cycle stability.

Description

technical field [0001] The invention relates to a method for preparing lithium manganese phosphate lithium / carbon as a lithium ion battery material by using sol-gel, and belongs to the technical field of new energy materials. Background technique [0002] Cathode materials are an important part of lithium-ion secondary batteries, currently mainly LiCoO 2 , LiNiO 2 , LiMn 2 o 4 Wait. LiCoO 2 High toxicity, high price, and certain safety problems; LiNiO 2 Low cost and high capacity, but difficult to prepare, poor thermal stability and material reproducibility, and serious safety problems; spinel LiMn 2 o 4 The cost is low, the safety performance is good, but the capacity is low, and the cycle performance, especially the high temperature cycle performance, is poor. Therefore, the development of positive electrode materials with excellent performance has become one of the hot fields in the research of lithium-ion battery materials. [0003] In recent years, phosphates h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/1397
CPCY02E60/122Y02E60/12Y02E60/10
Inventor 刘学武李新杨新刘贵昌
Owner DALIAN UNIV OF TECH
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