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Preparation method of lithium iron phosphate material

A lithium iron phosphate, lithium source technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems affecting the reduction degree of ferric salt, affecting the specific capacity, processing performance and cycle performance of lithium iron phosphate. problems such as large-scale production of lithium iron phosphate materials, to achieve the effect of shortening sintering time, good repeatability, and reducing energy consumption

Inactive Publication Date: 2013-08-21
郑州瑞普生物工程有限公司
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the methods for preparing lithium iron phosphate materials include high-temperature solid-phase method, liquid-phase precipitation method, hydrothermal method and microwave heating method, etc., but in actual production, high-temperature solid-phase method is mostly used, that is, two kinds of ferrous salt and lithium salt. Or two or more solid powder raw materials, the materials are mixed by mechanical ball milling and then calcined at high temperature. Since this method can only mix the materials to the micron level, if ferric orthophosphate is used as the raw material, this level of mixing will affect the ferric iron. The reduction degree of salt affects the specific capacity, processing performance and cycle performance of the final product of lithium iron phosphate, so the large-scale production of lithium iron phosphate materials is limited

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Weigh 363 g LiCO 3 , 1869 g FePO 4 2H 2 0 and 112 grams of glucose were mixed and ball milled to obtain a mixed powder (particle size D50 was 3-5 μm); 4.5 liters of deionized water was weighed and added to a wet ball mill, 225 grams of polyethylene glycol was added, and ball milled for 30 minutes with stirring, Get the polyethylene glycol solution; add the above mixed powder into the polyethylene glycol solution, wet ball mill for 4 hours (the minimum wet milling time should not be less than 1 hour), transfer to the NNM05 sand mill for nanometerization Treat for 150 minutes to obtain a mixed slurry with a particle size D50 of 200-500nm; spray-dry the above-mentioned mixed slurry through a GZ-5 spray drying equipment into particles with a particle size of about 10 μm-20 μm to obtain a lithium iron phosphate precursor; The lithium iron precursor was sintered at 600°C for 5 hours under the protection of a nitrogen atmosphere, and the sintered product was pulverized by a ...

Embodiment 2

[0023] Weigh 379 g LiCO 3 , 1869 g FePO 4 2H 2 O and 225 grams of glucose were mixed and ball-milled to obtain a mixed powder (particle size D50 is 3-5 μm); 5 liters of deionized water was weighed and added to a wet ball mill, 100 grams of polyethylene glycol was added, and ball milled for 30 minutes with stirring; Obtain polyethylene glycol solution; add the above-mentioned mixed powder into the polyethylene glycol solution, wet ball mill for 6 hours, transfer to NNM05 type sand mill for nano treatment for 90min, and obtain a particle size D50 of 200-500nm Mixed slurry; the above mixed slurry is spray-dried by GZ-5 spray drying equipment into particles with a particle size of about 10 μm-20 μm to obtain a lithium iron phosphate precursor; the above lithium iron phosphate precursor is carried out under the protection of an argon atmosphere After sintering at 700°C for 8 hours, the sintered product was pulverized by a ball mill to obtain a lithium iron phosphate product. The...

Embodiment 3

[0025] Weigh 449 grams of LiOH·H2O, 1869 grams of FEPO4·2H2O and 350 grams of sucrose, mix and ball mill to obtain a mixed powder (particle size D50 is 3-5 μm); weigh 8 liters of deionized water and add it to the wet ball mill, add 160 grams of polyethylene glycol were stirred and ball milled for 30 minutes; polyethylene glycol solution was obtained; the above mixed powder was added to the polyethylene glycol solution, wet ball milled for 8 hours, and then transferred to the NNM05 sand mill for nanometer chemical treatment for 50 minutes to obtain a mixed slurry with a particle size D50 of 200-500nm; the above-mentioned mixed slurry was spray-dried into particles with a particle size of about 10 μm-20 μm by a GZ-5 spray drying equipment to obtain a lithium iron phosphate precursor; The lithium iron phosphate precursor is sintered at 800°C for 8 hours under the protection of cracked ammonia atmosphere, and the sintered product is ball milled or pulverized to obtain the lithium i...

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Abstract

The invention discloses a preparation method of a high-tap density lithium iron phosphate material. The method comprises the following steps: mechanically mixing iron orthophosphate, a lithium source and a composite carbon source, transferring to a wet stirring ball milling device, adding a certain amount of deionized water and dispersant to form uniform suspension liquid, carrying out nano-ball milling on the obtained suspension liquid, spray-drying to obtain a precursor, and firing and crushing the obtained precursor to obtain the high-tap density lithium iron phosphate material. The lithium iron phosphate material prepared by the method disclosed by the invention has the characteristics of good processability, excellent electrochemical properties and the like when being used as a positive pole material of a lithium ion battery, and the preparation method is low in production cost, free of exhaust pollution, and convenient for commercial mass production.

Description

technical field [0001] The invention relates to a positive electrode material of a lithium ion secondary battery, in particular to a preparation method of a lithium iron phosphate material which can be used as a positive electrode material of a power type lithium ion battery. Background technique [0002] Since the advent of lithium-ion batteries, they have been widely used in some portable electronic products such as mobile phones, cameras, UPS power supplies, and notebook computers due to their light weight, high voltage, high energy density, and good cycle performance. In recent years, with the attention of various countries to the environment, energy and other issues, more and more lithium-ion batteries have also been used in electric vehicles. In lithium-ion battery systems, cathode materials play an important role. There are many kinds of positive electrode materials for lithium-ion batteries. At present, the large-scale commercial lithium battery positive electrod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/1397C01B25/45
CPCY02E60/10
Inventor 孙彦军江慧芳李良玉
Owner 郑州瑞普生物工程有限公司
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