Method for preparing anode material iron phosphate lithium of lithium ion battery

A lithium-ion battery, lithium iron phosphate technology, applied in electrode manufacturing and other directions, can solve problems such as inability to achieve mass production, complex liquid phase co-deposition process, and poor lithium ion conductivity.

Active Publication Date: 2008-02-06
龚思源
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  • Abstract
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  • Application Information

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Problems solved by technology

The advantage of the high-temperature method is that the process is simple and it is easy to realize industrialization, but the reactants are usually mixed unevenly, the product particles and grains are easy to grow, and the purity is not high. Therefore, the electrochemical performance is not high
The process of liquid phase co-deposition method is relatively complicated, Fe 2+ easily oxidized to Fe 3+ , need to add reducing agents such as ascorbic acid, the cost is high, and it is not conducive to industrialization
The sol-gel method can achieve molecular-level mixing of iron, phosphate and lithium, and it is also easy to achieve doping, and the properties of the obtained materials are also relatively ideal, but the process is relatively complicated and is not suitable for large-scale production
High-energy ball milling method (CN1255888C, Electrochem Solid State Lett 7 (2004) A522) mix metal iron powder, iron phosphate, lithium phosphate, doping element phosphate, conductive agent or conductive agent precursor in proportion, and place in an inert atmosphere. In a ball mill container, high-energy ball mill for 18-36 hours; the obtained ball mill product is put into a high-temperature furnace, and fired at a constant temperature of 450-750°C for 10-60min in an inert atmosphere such as nitrogen or argon, and the obtained lithium iron phosphate powder or doped phosphoric acid Lithium iron powder, the crystallinity of this positive electrode material is not very good, the conductivity of lithium ions is not good when charging and discharging at a high rate, and mass production cannot be realized

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  • Method for preparing anode material iron phosphate lithium of lithium ion battery

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Embodiment 1

[0022] A preparation method of lithium iron phosphate, a cathode material for lithium ion batteries, uniformly mixing lithium dihydrogen phosphate and ferrous oxide, controlling the molar ratio of phosphorus, iron and lithium in the raw materials to be 1.0:1.0:1.0, and using argon as a protective atmosphere , heating up to 850°C within 5 hours, keeping the temperature for 3 hours, and then cooling to room temperature to obtain a pure phase of lithium iron phosphate;

[0023] In the pure phase of lithium iron phosphate, add 9% conductive agent precursor sucrose by weight ratio of lithium iron phosphate and dropwise add 1% dilute sulfuric acid (30%) by weight ratio of lithium iron phosphate, fully mix and dry, and then use according to The weight ratio of lithium iron phosphate is 60% φ5mm and 40% φ20mm zirconia as the medium for ball milling for 18 hours;

[0024] Heat treatment at 580°C with argon as a protective atmosphere for 1 hour, and the output is lithium iron phosphate,...

Embodiment 2

[0028] A preparation method of lithium iron phosphate, a positive electrode material for lithium ion batteries, uniformly mixing lithium phosphate and ferrous phosphate, controlling the molar ratio of phosphorus, iron and lithium in the raw materials to be 1.0:0.85:1.00, heating in argon for 3 hours Raise the temperature to 950°C, sinter at constant temperature for 1.5 hours, and then naturally cool to obtain gray lithium iron phosphate powder;

[0029] What obtained is lithium iron phosphate and 5% conductive carbon black and 4% dilute hydrochloric acid (20%) after fully mixing and drying, then carry out ball milling with 30% φ5mm and 70% φ50mm agate balls for 30 hours;

[0030] Heat treatment in argon at 650°C for 2 hours, and the output is the cathode material lithium iron phosphate.

Embodiment 3

[0032]A preparation method of lithium iron phosphate, a positive electrode material for a lithium ion battery, uniformly mixes lithium hydroxide and dihydrogen phosphate ammonium ferrous ammonium, controls the molar ratio of phosphorus, iron and lithium in the raw materials to be 1.0:0.95:1.00, and uses hydrogen Argon is used as a protective atmosphere, and hydrogen and argon are used as a protective atmosphere to raise the temperature to 800°C within 6 hours and keep the reaction for 5 hours to obtain lithium iron phosphate powder;

[0033] What is obtained is lithium iron phosphate, 10% starch and 4% dilute nitric acid (15%) are fully mixed and dried, and then ball milled for 10 hours with 50% φ10mm and 50% φ30mm iron balls;

[0034] Heat treatment at 700°C with hydrogen and argon as a protective atmosphere for half an hour, and the output is the positive electrode material lithium iron phosphate.

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Abstract

The present invention relates to a method for producing LiFePO4 of positive pole of lithium ion battery. The invention is prominently characterized in that the method comprises three steps as follows: mixing the iron material, the lithium material and the phosphorus material uniformly to compound highly crystallized LiFePO4 in a high temperature first; adding a little diluted acid in the LiFePO4, after mixing and drying the processed LiFePO4 and conductive agent or pre-conductive agent, conducting ball mill for the mixture using a heavy ball; processing the mixture at a lower temperature and then the positive material LiFePO4 with excellent electrochemical performance can be gained. The gained LiFePO4 has favorable crystallinity and the electronic and the lithium ion conducting net is unique with excellent performance. The present invention uses cheap chemical product as raw material and the compounding art is simple thus is easy for producing on scale. The electrochemical character is favorable.

Description

technical field [0001] The invention relates to a preparation method of a cathode material of a lithium ion battery, in particular to a method for preparing lithium iron phosphate, an anode material of a lithium ion battery, by adopting high-temperature reaction, micro-acid dissolution, ball milling with heavy balls as a medium, and low-temperature lattice repair. Background technique [0002] Due to the advantages of high energy density, long service life, light weight, small self-discharge, no memory effect, and environmental friendliness, lithium-ion batteries have developed rapidly since their inception, and have become a popular choice for portable electronics such as mobile communications, notebook computers, and cameras. It is the preferred power source for products, and has been gradually developed as a power source for electric vehicles, defense equipment, etc., which also promotes the development of lithium-ion batteries in the direction of high energy, environmenta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/04
CPCY02E60/12Y02E60/10
Inventor 龚思源刘红仙黄强
Owner 龚思源
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