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Method for preparing carbon-coated lithium iron phosphate by one-step hydrothermal method

A technology of carbon-coated lithium iron phosphate and hydrothermal method, which is applied in the direction of active material electrodes, electrical components, electrochemical generators, etc., can solve the problems of affecting the electrical properties of materials, reducing production efficiency, increasing process flow, etc., to achieve Effects of suppressing particle size and agglomeration, saving time and cost, and reducing particle size

Active Publication Date: 2017-09-22
RIZHAO HUAXUAN NEW ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although the above-mentioned process has obtained carbon-coated lithium iron phosphate, there are still the following technical problems: ① The main function of the high-temperature sintering in the second step in the prior art is only to carry out carbon coating, which increases production costs and reduces production efficiency, which is not conducive to The promotion of the process of preparing carbon-coated lithium iron phosphate by hydrothermal method; ② During the mixing process of carbon-free lithium iron phosphate in carbon coating and carbon source ball milling, it will cause damage to the surface structure of lithium iron phosphate and affect the electrical properties of the material. The carbon source cannot be evenly coated on the surface of the particles, which will also affect the electrical properties of the material; ③ in the process of preparing lithium iron phosphate, it is necessary to control the size of the generated lithium iron phosphate particles. In terms of electrical properties, the size of lithium iron phosphate particles is usually controlled by adjusting the reaction temperature and adding surfactants; this not only increases the process flow, but also increases the difficulty of operation

Method used

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  • Method for preparing carbon-coated lithium iron phosphate by one-step hydrothermal method
  • Method for preparing carbon-coated lithium iron phosphate by one-step hydrothermal method
  • Method for preparing carbon-coated lithium iron phosphate by one-step hydrothermal method

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Experimental program
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Effect test

Embodiment 1

[0035] (1) First weigh 3.0 moles of LiOH and dissolve it in deionized water to form a 1.2 mol / L solution. After heating to 60°C, add 100 g of soluble starch and stir until it is completely gelatinized;

[0036] (2) Add the phosphoric acid of molar ratio Li:P=3.0:1.0 in the mixed slurry gained in step 1 again, i.e. 1 mole of phosphoric acid, keep warm at 80 ℃, keep stirring, obtain Li 3 PO 4 Suspension: due to the gelatinization of soluble starch added to the hot LiOH solution, the starch molecules in the granules stretch and diffuse in all directions, dissolve out of the granule, and expand Starch molecules are interconnected and entangled to form a network of hydrocolloids. When the starch enters the granule disintegration stage of the gelatinization reaction, the viscosity of the solution is the largest, which enables the starch molecules to wrap around LiOH, inhibits the reaction rate of LiOH and phosphoric acid, and inhibits the formation of Li 3 PO 4 The particle size ...

Embodiment 2

[0041] (1) First weigh 3.3 moles of LiOH and dissolve it in ionized water to form a 1.5 mol / L solution, add 120 g of water-soluble starch at room temperature, and stir until completely dissolved to form a mixed solution;

[0042] (2) Add the phosphoric acid of molar ratio Li:P=3.3:1.0 in the mixed liquor of gained in step 1 again, i.e. 1 mole of phosphoric acid, continuous stirring has generated Li 3 PO 4 Suspension; Li 3 PO 4 Add the suspension into the reaction kettle, seal the reaction kettle, use high-purity argon to purge the reaction kettle through the inlet valve, and discharge the internal air;

[0043] (3) take again the ferrous sulfate of Fe:P=1.0:1.0, i.e. 1 mole of ferrous sulfate, add in the deionized water of 0.5L, stir and dissolve, feed to Li through feed valve 3 PO 4 FeSO was added to the suspension 4 solution. The ratio of the added substances is the molar ratio Li: Fe: P = 3.1: 1.0: 1.0, the temperature of the reactor is raised to 240°C, and the temper...

Embodiment 3

[0046] (1) First weigh 3.1 moles of LiOH and dissolve it in deionized water to form a 1.0 mol / L solution, add 100 g of pregelatinized starch at 40°C, and stir until completely dissolved to form a starch paste;

[0047] (2) Add phosphoric acid with a molar ratio of Li:P=3.1:1.0 to the mixed solution obtained in step 1, that is, 1 mole of phosphoric acid, and stir at 40°C to form Li 3 PO 4 Suspension; Li 3 PO 4 The suspension is mixed with ultrasound at a frequency of 200Hz. The ultrasound makes the air bubbles in the mixture vibrate under the action of sound waves. When it reaches a certain limit, it will grow and collapse to play a role of cavitation. Using the effect of ultrasonic cavitation, Li 3 PO 4 Mix evenly with starch molecules in solution and control Li 3 PO 4 Particle size, uniform distribution. The Li after ultrasonic mixing 3 PO 4 Add the suspension into the reaction kettle, seal the reaction kettle, use high-purity argon to purge the reaction kettle throug...

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Abstract

The invention discloses a method for preparing carbon-coated lithium iron phosphate through a one-step hydrothermal method, and belongs to the field of lithium ion secondary battery anode materials. The preparation method solves the problems that a traditional carbon coating process is complex, a carbon-coating layer is not uniform, production cost is high, and electrochemical properties of products are not stable. The method is characterized in that carbon coating is completed in the hydrothermal synthesizing process, a lithium hydroxide starch paste mixture reacts with phosphoric acid to generate lithium phosphate suspension, the generated lithium phosphate suspension is mixed with a ferrite solution and reacts with the ferrite solution in a high-temperature reaction still in the inert atmosphere, the reaction temperature and time are controlled, and filtering, washing, drying and screening are conducted after the reaction ends so that carbon-coated lithium iron phosphate can be obtained. Compared with the prior art, the method has the advantages of being simple in process, low in cost, uniform in carbon-coated lithium iron phosphate granularity distribution, uniform in carbon-coating layer thickness and good in electrochemical performance.

Description

technical field [0001] The invention relates to the field of anode materials for lithium ion secondary batteries, in particular to a preparation method for lithium iron phosphate. Background technique [0002] Lithium iron phosphate battery has the advantages of non-toxic, non-polluting, good safety performance, wide source of raw materials, cheap price, long life, etc. It is the most ideal cathode material for the latest generation of power lithium-ion batteries. However, the lithium iron phosphate material has obvious shortcomings such as low electronic and ion conductivity, which limits the commercial development of this material to a certain extent. [0003] In order to improve the electronic conductivity and lithium ion diffusion coefficient of lithium iron phosphate, one of the methods is to reduce the particle size and reduce the diffusion path of Li ions inside the particles. However, since most of the existing lithium iron phosphate production processes are high-te...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/58
CPCH01M4/366H01M4/5825H01M4/625H01M10/0525H01M2004/021H01M2004/028Y02E60/10
Inventor 王海峰
Owner RIZHAO HUAXUAN NEW ENERGY