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A kind of microwave synthesis method of nano-lithium iron phosphate

A lithium iron phosphate, microwave synthesis technology, applied in the direction of phosphorus compounds, nanotechnology, chemical instruments and methods, etc., can solve the problems of limited phase purity, large power consumption, high cost, etc., to shorten the production cycle, save energy, particle uniform effect

Inactive Publication Date: 2011-12-14
IRICO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] But at present, the preparation of most lithium iron phosphate cathode materials is mostly prepared by solid-state method sintering, and then it is ball milled and mixed with carbon for carbon coating to increase the conductivity of lithium iron phosphate. In fact, , the particle size of the lithium iron phosphate prepared by the solid-state method is relatively large, and the carbon cannot be directly mixed and evenly coated on the outside of the lithium iron phosphate particle. Secondly, even if the lithium iron phosphate with a smaller particle size is obtained by crushing, Carbon cannot be fully covered around lithium iron phosphate particles
Its conductivity is still limited, and on the one hand, the particle size obtained by the crushing method is uneven, and the efficiency is low, and secondly, it is easy to damage the structure of the material, which fundamentally determines its poor conductivity.
At the same time, whether the current lithium iron phosphate method is solid-phase or liquid-phase, most of them are sintered in a high-temperature sintering furnace for a long time. During the sintering process, the raw materials are heated unevenly, the purity of the phase is limited, and the power consumption is huge. higher cost

Method used

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  • A kind of microwave synthesis method of nano-lithium iron phosphate
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] aWeigh 1molFeSO according to the molar ratio of 1:1 4 , 1molH 3 PO 4 (calculated by the effective content of phosphoric acid at 85% concentration), be dissolved in 2000ml of deionized water, then add 0.1mol complexing agent ethylene glycol, under constant stirring, slowly add 3000ml of 3mol lithium hydroxide solution to form mixed solution A;

[0021] b. Continuously stir the mixed solution A obtained in step a in an oil bath at 110° C. for 1 h until a green precipitate is produced, and the green precipitate is suction-filtered and washed to obtain a solid product;

[0022] c. Dry the solid product obtained in step b at 40° C. for 2 hours in a microwave vacuum dryer to obtain a precursor, and then perform ball milling on the precursor to obtain a spare precursor powder with a particle size of 20 nm;

[0023] d Put the standby precursor powder and high molecular polymer solution obtained in step c into a closed vacuum container, and then add a heat conducting agent, wh...

Embodiment 2

[0026] aWeigh 1molFeSO according to the molar ratio of 1:1 4 , 1molH 3 PO 4 (according to the effective content calculation of 85% concentration phosphoric acid), be dissolved in the deionized water of 2000ml, then add 0.1mol complexing agent triethanolamine, under constantly stirring, slowly add the lithium hydroxide solution 3000ml of 3mol, form mixed solution A;

[0027] b. The mixed solution A obtained in step a was continuously stirred in an oil bath at 130°C for 1.5h until a green precipitate was produced, and the green precipitate was subjected to suction filtration and washed to obtain a solid product;

[0028] c. Dry the solid product obtained in step b in a microwave vacuum dryer at 50° C. for 1.5 h to obtain a precursor, and then perform ball milling on the precursor to obtain a spare precursor powder with a particle size of 35 nm;

[0029] d Put the standby precursor powder and high molecular polymer solution obtained in step c into a closed vacuum container, and...

Embodiment 3

[0032] aWeigh 1molFeSO according to the molar ratio of 1:1 4 , 1molH 3 PO 4 (according to the effective content calculation of 85% concentration phosphoric acid), be dissolved in the deionized water of 2000ml, then add 0.1mol complexing agent polypropylene, under constantly stirring, slowly add the lithium hydroxide solution 3000ml of 3mol, form mixed solution A;

[0033] b. The mixed solution A obtained in step a was continuously stirred in an oil bath at 140°C for 2 hours until a green precipitate was produced, and the green precipitate was subjected to suction filtration and washed to obtain a solid product;

[0034] c. Drying the solid product obtained in step b at 60° C. for 1 h in a microwave vacuum dryer to obtain a precursor, and then performing ball milling on the precursor to obtain a spare precursor powder with a particle size of 50 nm;

[0035]d Put the standby precursor powder and high molecular polymer solution obtained in step c into a closed vacuum container,...

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Abstract

The invention provides a microwave synthesis method of nano-lithium iron phosphate. The method mainly makes the primary particles nanometerized, the secondary particles micronized, and then performs rapid sintering and synthesis through microwaves to obtain nanometer lithium iron phosphate with uniform phase. On the one hand, it solves the disadvantages of the uneven particle size of the solid-phase method, and can achieve molecular-level mixing to obtain products with uniform particle size, achieve nanometerization of primary particles, micronization of secondary particles, and improve ion transmission rate, thereby improving its electrical conductivity. . On the other hand, through microwave sintering, the raw materials are evenly heated to obtain nano-lithium iron phosphate with uniform phase, and the sintering time is greatly reduced, saving a lot of resources and achieving the purpose of energy saving and emission reduction.

Description

technical field [0001] The invention relates to a preparation method of a positive electrode material of a lithium ion battery, in particular to a microwave synthesis method of nanometer lithium iron phosphate. Background technique [0002] In lithium-ion batteries, the cathode material is the most important component and the key to determining the performance of lithium-ion batteries. Lithium iron phosphate materials have the characteristics of good safety, excellent cycle performance, environmental friendliness, and wide sources of raw materials. Among them, lithium, iron, and phosphorus are all elements with abundant reserves on the earth, especially iron-based materials, which have a wide range of raw materials and low prices. It is recognized as the preferred cathode material for a new generation of lithium-ion batteries, and has become the key research and development direction of major developed countries in the world today. Moreover, due to the stability of itself a...

Claims

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Application Information

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IPC IPC(8): C01B25/45B82Y40/00
Inventor 王少卿
Owner IRICO
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