Hydrothermal synthesis method for positive pole material lithium manganese phosphate nanoparticles of lithium-ion batteries

A hydrothermal synthesis method, a technology for lithium ion batteries, applied in battery electrodes, phosphorus compounds, nanotechnology, etc., can solve the problems of slow lithium ion diffusion, unseen, poor conductivity, etc., to improve high current charge and discharge performance , Easy to scale production, low cost effect

Inactive Publication Date: 2014-12-03
ZHEJIANG UNIV
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  • Summary
  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

The study found that the lithium manganese phosphate material has a moderate working voltage (4.1V), a theoretical capacity of 171mAh / g, good cycle performance, and low cost, and its energy density is 34% higher than that of lithium iron phosphate. Its high energy density and high The safety performance makes it have outstanding application prospects in power lithium-ion batteries, but its disadvantages are its poor conductivity and slow diffusion of lithium ions, which are greatly related to the particle size of lithium manganese phosphate cathode materials
The present invention uses a simple method to prepare the lithium manganese phosphate positive electrode material with a carbon layer with a smaller size, which is conducive to improving battery performance, and has not yet seen such a block copolymer as a template agent and potassium hydroxide as a mineralization agent. Preparation of lithium manganese phosphate nanoparticles by the hydrothermal method

Method used

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  • Hydrothermal synthesis method for positive pole material lithium manganese phosphate nanoparticles of lithium-ion batteries

Examples

Experimental program
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Effect test

example 1

[0022] 1) Dissolve 2.00 g of P123 in 20 ml of deionized water, stir for 240 minutes, then add 3.38 g of manganese sulfate and 0.20 g of ascorbic acid, stir until fully dissolved, and obtain a manganese source concentration of 1.0 mol / L and an ascorbic acid concentration of 0.076 mol / L L, a solution A with a templating agent concentration of 0.1 g / mL;

[0023] 2) Dissolve 1.96g of phosphoric acid and 2.56g of lithium sulfate in 20 ml of deionized water and stir for 30 minutes to form a suspension B with a phosphoric acid concentration of 1.0 mol / L and a lithium source concentration of 1.0 mol / L;

[0024] 3) Add the suspension B prepared in step 2) dropwise to the solution A prepared in step 1) under stirring to form emulsion C. The molar ratio of Li, Mn, and P in emulsion C is 1:1:1.

[0025] 4) Transfer the emulsion C in step 3) to a 60ml autoclave, add 0.112 g of KOH, stir well, and then adjust its volume to 40ml with deionized water, so that the concentration of KOH is 0.05...

example 2

[0028] 1) Dissolve 4.00 g of P123 in 20 ml of deionized water, stir for 240 minutes, then add 6.76 g of manganese sulfate and 0.40 g of ascorbic acid, stir until fully dissolved, and obtain a manganese source concentration of 2.0 mol / L and an ascorbic acid concentration of 0.152 mol / L L, the solution A whose template concentration is 0.2 g / mL;

[0029] 2) Dissolve 3.92g of phosphoric acid and 3.36g of lithium hydroxide in 20 ml of deionized water and stir for 30 minutes to form a suspension B with a phosphoric acid concentration of 2.0 mol / L and a lithium source concentration of 4.0 mol / L;

[0030] 3) Add the suspension B prepared in step 2) dropwise to the solution A prepared in step 1) under stirring to form emulsion C. The molar ratio of Li, Mn, and P in emulsion C is 2:1:1.

[0031] 4) Transfer the emulsion C in step 3) to a 50ml autoclave, add 0.224g of KOH, stir well, then adjust its volume to 40ml with deionized water, so that the concentration of KOH is 0.10 mol / L, an...

example 3

[0034] 1) Dissolve 3.00 g of F127 in 20 ml of deionized water, stir for 240 minutes, then add 5.94 g of manganese chloride and 0.32 g of ascorbic acid, stir until fully dissolved, and obtain a manganese source concentration of 1.5 mol / L and an ascorbic acid concentration of 0.091 mol / L, the template concentration is solution A of 0.15 g / mL;

[0035] 2) Dissolve 2.94g of phosphoric acid and 3.78g of lithium hydroxide in 20 ml of deionized water and stir for 30 minutes to form a suspension B with a phosphoric acid concentration of 1.5 mol / L and a lithium source concentration of 4.5 mol / L;

[0036] 3) Add the suspension B prepared in step 2) dropwise to the solution A prepared in step 1) under stirring to form emulsion C. The molar ratio of Li, Mn, and P in emulsion C is 3:1:1.

[0037] 4) Transfer the emulsion C in step 3) to a 60ml autoclave, add 0.336g of KOH, stir well, then adjust its volume to 40ml with deionized water, so that the concentration of KOH is 0.15 mol / L, and ...

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Abstract

The invention discloses a hydrothermal synthesis method for positive pole material lithium manganese phosphate nanoparticles of lithium-ion batteries. According to the hydrothermal synthesis method, deionized water serves as a solvent, a manganese source, a lithium source and phosphoric acid are taken as reacting materials, a block copolymer is taken as a template agent, potassium hydroxide is taken as a mineralizer, so as to promote nucleation and growth of lithium manganese phosphate, heat treatment is carried out at high temperature and high pressure, then, calcining treatment is carried out at the temperature of 550-650 DEG C under the protection of a nitrogen or argon atmosphere while carrying out heat preservation, and then, the lithium manganese phosphate nanoparticles are obtained. The hydrothermal synthesis method has the advantages that the product is stable in quality, high in purity and good in particle dispersibility and is beneficial to the diffusion of lithium ions and the improvement of the electrochemical properties of a lithium-ion battery, and the preparation process is simple in process, easy to control and low in cost and is pollution-free, so that the large-scale production is facilitated.

Description

technical field [0001] The invention relates to a preparation method of lithium manganese phosphate, a cathode material of a lithium ion battery, in particular to a hydrothermal synthesis method of lithium manganese phosphate nanoparticles. Background technique [0002] Lithium-ion battery is a new type of battery after nickel-cadmium and nickel-metal hydride batteries. Due to the advantages of high working voltage, small size, and light weight, lithium-ion batteries have been widely used in various portable electronic products and communication tools in recent years, and have been gradually developed as power sources for electric vehicles. [0003] At present, extensive research on cathode materials for lithium-ion batteries focuses on transition metal oxides of lithium such as LiMO with a layered structure. 2 (M=Co, Ni, Mn) and LiMn with spinel structure 2 o 4 . However, they have their own disadvantages as cathode materials, LiCoO 2 High cost, poor resources, high to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58C01B25/45B82Y40/00
CPCB82Y40/00C01B25/45H01M4/5825H01M10/0525Y02E60/10
Inventor 徐刚李玲玲李峰任召辉刘涌李翔沈鸽韩高荣
Owner ZHEJIANG UNIV
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