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Doped modified lithium iron phosphate and preparation method thereof

A lithium iron phosphate, modified technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of difficulty in improving high-current discharge, difficulty in LiFePO, uneven battery performance, etc. Excellent chemical properties, no three-waste emissions, and the effect of clean industrialized large-scale production

Inactive Publication Date: 2013-01-16
绵阳天明新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] As we all know, compared with other mainstream cathode materials, Lithium Ferrous Phosphate has the disadvantage of weak electrical conductivity, which will directly lead to the poor performance of batteries based on this material under charge and discharge. The deintercalation and movement of lithium ions in the system are hindered, and the utilization rate of active materials is low. For the research of lithium iron phosphate lithium iron phosphate in power batteries, it is very important and difficult to improve its high-current discharge. Therefore, the improvement methods in the industry are mainly to add conductive agents during the material synthesis process, or to use particle coating methods to coat conductive substances on the surface of lithium iron phosphate particles in the later stage, so that the materials have relatively good Conductivity, when the battery is made, a certain amount of conductive agent is also added according to the ratio
The current technology suffers from the following disadvantages, which hinder its practical application:
[0003] (1) Fe2+ in the synthesis is easily oxidized to Fe3+, and it is not easy to obtain single-phase LiFePO4;
[0004] (2) Diffusion of lithium ions in LiFePO4 is difficult, resulting in low utilization of active materials;
[0005] (3) The conductivity of LiFePO4 itself is also very low, resulting in poor high-current discharge performance;
[0006] (4) In the process of material application, due to the error caused by multiple conductive agent additions, the final battery performance is uneven, which reduces the consistency of the product

Method used

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  • Doped modified lithium iron phosphate and preparation method thereof
  • Doped modified lithium iron phosphate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A preparation method for doping modified lithium iron phosphate, such as figure 1 process, follow the steps below:

[0035] 1. Weigh according to the raw material formula indicated in Table 1;

[0036] 2. Put the weighed raw materials in 300ml of ethanol and mix evenly, then put the mixed materials in a ball mill container, and ball mill for 36 hours;

[0037] 3. Place the ball-milled product in an air atmosphere and dry at 110°C for 10 hours. After natural cooling, grind to a particle size of 80 mesh or more to obtain a uniformly mixed high-density precursor of lithium iron phosphate;

[0038] 4. Place the precursor of lithium ferrous phosphate obtained above in a high-temperature furnace, raise the temperature to 800°C at a heating rate of 60°C / h in a nitrogen atmosphere, and roast at a constant temperature of 800°C for 20 hours, then cool naturally to 80°C Below ℃, silver-doped lithium iron phosphate powder can be obtained.

[0039] The properties and paramete...

Embodiment 2

[0041] A preparation method for doping modified lithium iron phosphate, such as figure 1 process, follow the steps below:

[0042] 1. Weigh according to the raw material formula indicated in Table 1;

[0043] 2. Put the weighed raw materials in 300ml of water and mix evenly, then put the mixed materials in a ball mill container, and ball mill for 24 hours;

[0044] 3. Place the ball-milled product in an air atmosphere and dry it at 90°C for 20 hours. After natural cooling, grind it to a particle size of 80 mesh or more to obtain a uniformly mixed high-density precursor of lithium iron phosphate;

[0045] 4. Place the precursor of lithium ferrous phosphate obtained above in a high-temperature furnace, raise the temperature to 700°C at a heating rate of 50°C / h in a nitrogen atmosphere, and roast at a constant temperature of 700°C for 20 hours, then cool naturally to 80°C Below ℃, manganese-doped lithium iron phosphate powder can be obtained.

[0046] The properties and parame...

Embodiment 3

[0048] A preparation method for doping modified lithium iron phosphate, such as figure 1 process, follow the steps below:

[0049] 1. Weigh according to the raw material formula indicated in Table 1;

[0050] 2. Put the weighed raw materials in a mixture of 300ml ether and water (the molar ratio of ether and water is 1:1) and mix evenly, then put the mixed materials in a ball mill container and mill them for 30 hours;

[0051] 3. Place the ball mill product in an air atmosphere and dry it at 100°C for 15 hours. After natural cooling, grind it to a particle size of 80 mesh or more to obtain a uniformly mixed high-density precursor of lithium iron phosphate;

[0052] 4. Place the precursor of lithium ferrous phosphate obtained above in a high-temperature furnace, in a nitrogen atmosphere, heat up to 750°C at a heating rate of 55°C / h, roast at a constant temperature of 750°C for 18 hours, and then cool naturally to 80°C Below ℃, magnesium-doped lithium iron phosphate powder can...

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Abstract

The invention discloses a raw material formula of doped modified lithium iron phosphate. Components include a ferric iron source, a phosphorus source, a lithium source, a doped element compound and excess carbon sources, wherein the mole ratio of to ferric iron source to the phosphorus source to the lithium source to the doped element compound to the carbon sources is 1:1-1.05:1-1.1:0.01-0.05:0.1-0.2. A preparation method directly adopts the ferric iron source, so that a cockamamie step of synthesizing ferrous salt by means of other synthesizing technologies is avoided, and the problem that usual products produced by means of conventional preparation methods using a ferrous salt raw material oxidizable in the air are impure is solved. A synthesized doped modified lithium iron phosphate material is small in particle diameter, narrow in distribution, high in purity, large in compaction and excellent in electrochemistry performance. A synthesized positive pole material and a carbon negative pole are assembled to form a test battery, the specific capacity is more than 130mAh / g when discharging is performed in 1C multiplying power, and excellent circulating stability performance is displayed.

Description

technical field [0001] The invention relates to a raw material formula for preparing lithium ferrous phosphate and a preparation method thereof, belonging to the field of lithium battery electrode materials. Background technique [0002] As we all know, compared with other mainstream cathode materials, Lithium Ferrous Phosphate has the disadvantage of weak conductivity, which will directly lead to the hindering of lithium ion intercalation and movement in the system under charge and discharge of the battery based on this material, and the active material The utilization rate is low, and for the industry to devote itself to the research of lithium iron phosphate for power batteries, it is a very important and difficult lesson to improve its high-current discharge. Therefore, the improvement method in the industry is mainly in the material synthesis process. Add a conductive agent to the battery, or use the method of particle coating to coat the conductive substance on the sur...

Claims

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Application Information

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IPC IPC(8): H01M4/58C01B25/45
CPCY02E60/12Y02E60/10
Inventor 周天明左一村喻国强
Owner 绵阳天明新能源科技有限公司
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