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Preparation method of lithium iron phosphate of cathode material of lithium ion secondary battery

A technology of lithium iron phosphate and positive electrode materials, which is applied in the direction of battery electrodes, circuits, electrical components, etc., and can solve problems such as hindering the practical process, loss of initial capacity, poor performance of high-rate charge and discharge, and low tap density

Active Publication Date: 2011-10-05
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Although LiFePO 4 It has many advantages, but it also has the following two disadvantages that hinder its practical application: (1) low electronic conductivity and lithium ion diffusion rate, resulting in initial capacity loss and poor high-rate charge-discharge performance; (2) ) during the synthesis of LiFePO 4 It is difficult to control the purity of Fe, even if the synthesis conditions are strictly controlled, it is still impossible to completely avoid Fe 3+ is oxidized, and most of the researches currently use the more expensive Fe 3+ The compound is used as iron source, which increases the preparation cost
(3) LiFePO 4 The tap density is lower, resulting in a lower volume specific energy
However, it is difficult to design and manufacture large-scale high-temperature and high-pressure reactors, and the cost is high, and it is often necessary to add twice as much Li salt as a precipitant during the synthesis process, which increases the preparation cost
[0007] Patent CN200410017382.5 adopts low-priced ferric source and one-step solid phase synthesis of carbon-coated lithium iron phosphate simplifies the process and reduces the cost. Carbon coating can well solve the problem of poor conductivity of lithium iron phosphate , the 0.2C discharge capacity is 157mAh / g, but the conductivity inside the lithium iron phosphate lattice has not changed, and the 1C discharge capacity is 124mAh / g, which is still a long way from large-scale industrialization

Method used

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  • Preparation method of lithium iron phosphate of cathode material of lithium ion secondary battery
  • Preparation method of lithium iron phosphate of cathode material of lithium ion secondary battery
  • Preparation method of lithium iron phosphate of cathode material of lithium ion secondary battery

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Take 1500ml of deionized water, add 12 grams of polyacrylic acid, and then add 60 grams of carbon black, disperse and infiltrate for 12 hours.

[0030] Add the dispersed and infiltrated carbon black into the stirring mill, then add 523 grams of lithium dihydrogen phosphate, 393 grams of iron oxide, 14.5 grams of magnesium hydroxide, and 35.65 grams of sucrose, and stir for 3-5 hours.

[0031] The above mixture was diluted with deionized water and then spray-dried.

[0032] Take 50 grams of the spray-dried material and place it in a tube furnace to sinter at a rate of 2°C / min in a nitrogen atmosphere, keep it at 400°C for 4 hours, keep it at 600°C for 10 hours, keep it at 720°C for 15 hours, and then cool down to obtain Lithium iron phosphate composite cathode material.

[0033] The obtained positive electrode material is packed into a simulated battery, the diaphragm is celgard2400, the negative electrode is a metal lithium sheet, and the electrolyte is LiPF 6 (EC:DEC:D...

Embodiment 2

[0035] Take 1000ml of deionized water, add 4.8g of Tween 85, then add 24g of carbon black, disperse and infiltrate for 12 hours.

[0036] Add the dispersed and infiltrated carbon black into the stirring mill, then add 208.68 grams of lithium dihydrogen phosphate, 157.4 grams of iron oxide, 21.45 grams of magnesium acetate tetrahydrate, and 14.2 grams of sucrose. Stir for 3-5 hours.

[0037] The above mixture was diluted with deionized water and then spray-dried.

[0038] Take 30 grams of the spray-dried material and place it in a tube furnace for sintering at a rate of 2°C / min in a nitrogen atmosphere, keep it at 200°C for 3 hours, keep it at 400°C for 4 hours, keep it at 700°C for 15 hours, and then cool down to prepare Lithium iron phosphate composite cathode material was obtained.

[0039] The obtained positive electrode material is packed into a simulated battery, the diaphragm is celgard2400, the negative electrode is a metal lithium sheet, and the electrolyte is LiPF ...

Embodiment 3

[0041] Take 1300ml of deionized water, add 10g of polyacrylate ammonium salt, then add 50g of carbon black, disperse and infiltrate for 12 hours.

[0042] The dispersed and infiltrated carbon black was added to the stirring mill, and then 528 grams of lithium dihydrogen phosphate, 393 grams of iron oxide, 10 grams of magnesium oxide, and 37.7 grams of sucrose were added. Stir for 3-5 hours.

[0043] The above mixture was diluted and then spray-dried.

[0044] Take 50 grams of the spray-dried material and place it in a tube furnace to sinter at a rate of 2°C / min in a nitrogen atmosphere, keep it at 200°C for 4 hours, keep it at 400°C for 5 hours, keep it at 700°C for 12 hours, and then cool down to prepare Lithium iron phosphate composite cathode material was obtained.

[0045] The obtained positive electrode material is packed into a simulated battery, the diaphragm is celgard2400, the negative electrode is a metal lithium sheet, and the electrolyte is LiPF 6 (EC:DEC:DMC=1:...

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Abstract

The invention provides a preparation method of lithium iron phosphate of a cathode material of a lithium ion secondary battery, which comprises the following steps: well mixing a trivalent iron source, a carbon source, a phosphate source, a lithium source, and doped ions, performing working procedures such as drying and the like to obtain a lithium iron phosphate precursor mixture, heating the mixture in reducing atmosphere with a heating rate of 0.1-10 DEG C / min, calcining the mixture at 200-800 DEG C for 5-25 hours, cooling the mixture to room temperature in the furnace, grinding the mixture to obtain the cathode material of a lithium ion electrode. The preparation method has simple process, and low cost, and the prepared cathode material of a lithium electrode has good discharge and cycle performance; the process parameters are easy to control; the batch has good stability; and the preparation method is suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of preparation of positive electrode materials of lithium ion batteries, and in particular relates to a method for preparing lithium iron phosphate, a positive electrode material of lithium ion secondary batteries, by using a trivalent iron source. technical background [0002] Olivine LiFePO 4 Because of its low cost, environmental friendliness, long cycle life, good thermal stability and high safety performance, it is considered to be one of the best cathode materials for lithium-ion power batteries. [0003] Although LiFePO 4 It has many advantages, but it also has the following two disadvantages that hinder its practical application: (1) low electronic conductivity and lithium ion diffusion rate, resulting in initial capacity loss and poor high-rate charge-discharge performance; (2) ) during the synthesis of LiFePO 4 It is difficult to control the purity of Fe, even if the synthesis conditions are strictly cont...

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 陈海涛陈雷刘大军徐小明
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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