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Solvothermal method used for preparing LiFePO4

A solvothermal method and solution technology, applied in the field of solvothermal preparation of LiFePO4, can solve the problems of unsuitable high-rate discharge and large particle size, and achieve the effect of improving processing performance and compaction density

Inactive Publication Date: 2012-06-13
CHINA JILIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In numerous LiFePO 4 In the preparation method, the hydrothermal / solvothermal method is a very important method. Since the use of soluble materials as reactants makes the ions can be uniformly mixed during the synthesis process, thereby obtaining a better crystal form and a very pure phase , since the first synthesis of LiFePO by Shou-FengYang et al. 4 Since the material (Electrochemistry Communications, 2001, 3, 205.), the preparation of LiFePO by hydrothermal / solvothermal method 4 The material has been extensively studied, LiFePO synthesized by hydrothermal method 4 It has the disadvantages of large particle size and is not suitable for high rate discharge, but a large amount of small particle size LiFePO must be synthesized by solvothermal method 4 Materials have always been a difficult problem to solve

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  • Solvothermal method used for preparing LiFePO4
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  • Solvothermal method used for preparing LiFePO4

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Embodiment 1

[0027] The stoichiometric ratio of phosphoric acid and ferrous sulfate was dissolved in deionized water to prepare 0.1 mol / L clear solution A. Then prepare 0.3mol / L lithium hydroxide solution and add 0.05mol / L reducing agent N 2 H 4 , and stir to form a clear and homogeneous solution B. While vigorously stirring A, slowly add solution B to A, stir evenly to obtain a dark green suspension, and use deionized water to centrifuge and wash the obtained product three times to obtain amorphous LiFePO 4 precipitation. The obtained amorphous LiFePO 4Disperse in an appropriate amount of ethylene glycol, disperse uniformly by ultrasonic, then transfer to a hydrothermal reactor, and react at 200 ° C for 10 hours under constant stirring, and use deionized water, anhydrous alcohol, etc. for the obtained product. The product was washed several times and dried at 80°C under certain vacuum conditions to obtain LiFePO with good crystallization and a particle size of 5 μm. 4 ,like figure 1...

Embodiment 2

[0029] Dissolve ammonium monohydrogen phosphate and ferrous sulfate in the stoichiometric ratio in deionized water, adjust with dilute sulfuric acid to make it clear, and prepare a clear solution A of 0.05mol / L. Then prepare 0.05mol / L lithium sulfate solution and add 0.01mol / L reducing agent N 2 H 4 , and stir to form a clear and homogeneous solution B. While vigorously stirring A, slowly add solution B to A, stir evenly to obtain a dark green suspension, centrifuge and wash the obtained product three times with deionized water to obtain amorphous LiFePO 4 . The obtained amorphous LiFePO 4 Disperse in an appropriate volume ratio of 1:1 ethylene glycol / CCl 4 In the mixed solvent, ultrasonically dispersed uniformly, then transferred to a hydrothermal reactor, and reacted at 180 ° C for 20 hours under constant stirring, and the obtained product was washed several times with deionized water, anhydrous alcohol, etc. Dry at 80°C under vacuum to obtain nano-LiFePO4 with good cry...

Embodiment 3

[0031] Dissolve phosphoric acid and ferrous ammonium sulfate in the stoichiometric ratio in deionized water to prepare a 0.5mol / L clear solution A, then prepare a 0.3mol / L lithium hydroxide solution and add a reducing agent to a concentration of 0.05mol / L Reducing agent vitamin C, stir evenly to form a clear and homogeneous solution B. While vigorously stirring, solution B was slowly added to A, and stirred evenly to obtain a dark green suspension. The obtained product was centrifuged and washed three times with deionized water. The obtained amorphous LiFePO4 was dispersed in an appropriate amount of triethylene glycol / cyclohexane organic mixed solvent with a volume ratio of 1:1, and 2% by volume of the morphology regulator succinic acid was added, and a 1% by mass ratio of surface The active agent sodium lauryl sulfate was dispersed uniformly by ultrasonic, and then transferred to a hydrothermal reactor, and reacted at 240 ° C for 20 hours under constant stirring, and the obt...

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Abstract

The invention relates to a solvothermal method used for preparing LiFePO4 with adjustable particle size and controllable morphology. The prepared LiFePO4 can be used as an anode material for a high-rate lithium ion battery. The method comprises steps that: a soluble phosphorous source and divalent ferrite are dissolved in deionized water; lithium salt is uniformly mixed with a surfactant, a reducing agent, and the like; the two solutions are mixed, such that amorphous LiFePO4 is obtained; the amorphous LiFePO4 is subject to centrifugation; a morphology controlling agent is added to the amorphous LiFePO4, and the solution is stirred until the solution reaches a uniform, clarified and stable state; the solution is added into a reaction vessel, and is subject to a reaction for a certain amount of time under high temperature and high pressure; the material is subject to centrifugal washing and drying, such that LiFePO4 with adjustable morphology and size is obtained.

Description

technical field [0001] The invention relates to a preparation of LiFePO 4 The method, specifically, involves a preparation of LiFePO 4 solvothermal method. Background technique [0002] The energy problem in today's world cannot be ignored. The world is calling for energy-saving and environmentally friendly materials. In such a large environment, the development of electric vehicles has emerged as the times require, and the problems that need to be solved are concentrated on batteries. At present, the development of batteries is very competitive. There are many types of cathode materials for lithium-ion batteries, the main varieties are lithium cobalt oxide, lithium manganate, nickel manganese cobalt ternary materials and lithium iron phosphate (LiFePO 4 ), etc. Among them, lithium cobalt oxide is the most industrialized, most mature, and most productive cathode material among the existing cathode materials. It is mainly used in the field of small batteries such as mobile ...

Claims

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Application Information

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IPC IPC(8): H01M4/58
CPCY02E60/12Y02E60/10
Inventor 田光磊舒康颖王蕾范美强吕春菊秦来顺
Owner CHINA JILIANG UNIV
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