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Method for preparing lithium iron phosphate positive pole material through hydrothermal method

A lithium iron phosphate and cathode material technology, applied in chemical instruments and methods, phosphorus compounds, battery electrodes, etc., can solve the problems of wide particle size distribution, uneven particles, and high reaction temperature, to improve rate performance, reduce Effects of reaction temperature and high specific surface area

Inactive Publication Date: 2013-08-21
XIAN TECHNOLOGICAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention provides a method for preparing lithium iron phosphate positive electrode material by hydrothermal method, so as to overcome the problems of uneven particle size, irregular crystal form, wide range of particle size distribution, high reaction temperature, long synthesis period and low product quality in the prior art. The batch stability is poor, which affects the stability of material performance

Method used

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  • Method for preparing lithium iron phosphate positive pole material through hydrothermal method
  • Method for preparing lithium iron phosphate positive pole material through hydrothermal method
  • Method for preparing lithium iron phosphate positive pole material through hydrothermal method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Preparation of LiFePO by Hydrothermal Method 4 The method comprises the following steps in turn:

[0024] (1) First weigh 0.3mol Li0H and add deionized water to dissolve it in a 500ml beaker, then add 0.1molH 3 P0 4 Slowly add LiOH solution along the wall of the vessel, and centrifuge to obtain Li 3 P0 4 White precipitate, dried under vacuum at 50°C-60°C to obtain LiFePO 4 powder.

[0025] (2) Add in another beaker, and weigh Li respectively at a molar ratio of 1:3 3 PO 4 = 0.5891g; and (NH 4 ) 2 Fe(SO 4 ) 2 =1.9877g, M (glucose)=0.1660g is added deionized water and is dissolved in the beaker, after stirring evenly, add to the stainless steel reaction kettle, the filling amount of described mixed solution in the reaction kettle is 60%.

[0026] (3) Put it into the reaction kettle and heat it to 200°C, heat for 5 hours, cool to room temperature after the reaction, and take out the reaction kettle; use deionized water and detergent to separate the sediment thre...

Embodiment 2

[0028] (1) First weigh 0.3mol Li0H and add deionized water to dissolve it in a 500ml beaker, then add 0.1molH 3 P0 4 Slowly add LiOH solution along the wall of the vessel, and centrifuge to obtain Li 3 P0 4 White precipitate, dried under vacuum at 50°C-60°C to obtain LiFePO 4 powder.

[0029] (2) Add in another beaker, and weigh Li respectively at a molar ratio of 1:3 3 PO 4 = 0.5882g; and (NH 4 ) 2 Fe(SO 4 ) 2 =1.9802g, M (glucose)=0.1607g add deionized water and dissolve in the beaker, stir and add to the stainless steel reactor after stirring, the filling amount of the mixed solution in the reactor is 60%.

[0030] (3) Put it into the reaction kettle and heat it to 180°C, heat for 5 hours, cool to room temperature after the reaction, and take out the reaction kettle; use deionized water and detergent to separate the precipitate three times, and then use ethanol lotion for three times after centrifugal separation , dried under vacuum at 60°C to obtain LiFePO 4 pow...

Embodiment 3

[0032] Preparation of LiFePO by Hydrothermal Method 4 The method comprises the following steps in turn:

[0033] (1) First weigh 0.3mol Li0H and add deionized water to dissolve it in a 500ml beaker, then add 0.1molH 3 P0 4 Slowly add LiOH solution along the wall of the vessel, and centrifuge to obtain Li 3 P0 4 White precipitate, dried under vacuum at 50°C-60°C to obtain LiFePO 4 powder.

[0034] (2) Add in another beaker, and weigh Li respectively at a molar ratio of 1:3 3 PO 4 = 0.3671g; and (NH 4 ) 2 Fe(SO 4 ) 2 =1.2464g, M (glucose)=0.0848g add deionized water and dissolve in the beaker, add to the stainless steel reactor after stirring evenly, the filling amount of described mixed solution in the reactor is 60%.

[0035] (3) Put it into the reaction kettle and heat it to 160°C, heat it for 8 hours, cool to room temperature after the reaction, take out the reaction kettle; use deionized water and lotion to separate the sediment three times, and then use ethanol ...

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Abstract

The invention relates to a lithium ion battery positive pole material, and particularly relates to a method for preparing a lithium iron phosphate positive pole material through a hydrothermal method. The method aims at solving the problems of nonuniform granule, irregular crystal, wide size distribution range, high reaction temperature, long synthesis period, poor product batch stability and material property stability influence in the prior art. In order to solve the problems in the prior art, the technical scheme is as follows: the method for preparing the lithium iron phosphate positive pole material through the hydrothermal method sequentially comprises the following steps of: (1) weighing LiOH.H2O and 85% H3PO4, dissolving the LiOH.H2O into deionized water, slowly dripping strong phosphoric acid into an LiOH.H2O solution, centrifugalizing to obtain Li3PO4 white precipitates, and carrying out vacuum drying to obtain Li3PO4 powder; (2) weighing Li3PO4 and (NH4)2Fe(SO4)2.6H2O, adding the deionized water to dissolve in a beaker, adding reducing agent glucose at the same time, and uniformly stirring; and (3) reacting, then cooling to room temperature, carrying out microwave oscillation, centrifugalizing a lotion for separation, and drying to obtain LiFePO4 powder.

Description

technical field [0001] The invention relates to a lithium ion battery cathode material, in particular to a method for preparing a lithium iron phosphate cathode material by a hydrothermal method. Background technique [0002] The performance of lithium-ion batteries depends on the positive and negative electrode materials, LiFePO 4 As a battery cathode material, it has the advantages of high specific capacity, low raw material price, environmental friendliness, high safety, and good cycle performance, and has become the most potential lithium-ion power battery cathode material. Compared with traditional lithium cobalt oxide cathode materials, LiFePO 4 It also has the advantages of abundant sources, low cost, environmental friendliness and non-moisture absorption, high specific capacity, stable voltage platform, thermal stability and good cycle performance. [0003] The solid phase method is the current preparation of LiFePO 4 Commonly used methods, but it is difficult...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58C01B25/45H01M4/62
CPCY02E60/10
Inventor 郑德山张晓惠陈力
Owner XIAN TECHNOLOGICAL UNIV
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