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Preparation method of lithium iron phosphate as cathode material of lithium ion battery

A technology for lithium-ion batteries and cathode materials, which is applied in the field of preparation of cathode materials for lithium-ion batteries, can solve the problems of being unsuitable for large-scale production, low degree of product crystallization, and low purity of synthesized products, and achieve excellent electrochemical performance. The effect of excellent chemical performance and low cost

Active Publication Date: 2012-06-13
CHINA AUTOMOTIVE BATTERY RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Typical methods in high-temperature solid-phase synthesis include high-temperature synthesis methods using expensive ferrous organic compounds as precursors. In this method, ferrous iron will be oxidized even under the protection of an inert atmosphere, and the purity of the synthetic product Not high, low tap density; carbothermal reduction method with ferric iron as precursor, long synthesis time and high energy consumption
The advantage of the low-temperature liquid-phase synthesis method is that the mixing of raw materials can reach the molecular level, but the degree of crystallization of the product is not high, and there is a phenomenon of mixed displacement of Fe and Li, which still needs to be processed at high temperature, which complicates the preparation process and is not suitable for large-scale production.

Method used

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  • Preparation method of lithium iron phosphate as cathode material of lithium ion battery
  • Preparation method of lithium iron phosphate as cathode material of lithium ion battery
  • Preparation method of lithium iron phosphate as cathode material of lithium ion battery

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Mix 0.5 mole of iron powder, 0.5 mole of lithium dihydrogen phosphate, and 8% sucrose accounting for the total weight of the raw materials and put them into a rod mill jar, use ethanol as the medium, and fully mix them on the rod mill for 5 hours. Drying, the dried mixture is mechanically stirred and granulated with a polyvinyl alcohol solution of 5wt% relative to the total weight of the raw material, and the granulated mixture is put into a shaft furnace, under an argon atmosphere of 5 liters / min, at 6°C The temperature was raised to 300°C for 10 hours at a rate of 1 / min, then synthesized at 700°C for 20 hours, and then lowered to room temperature to obtain lithium iron phosphate. The measured tap density of the synthetic material is 1.43g / cm 3 . figure 1 For the synthesis product LiFePO 4 It can be seen from the scanning electron microscope photo that the particle size of the synthesized product is basically less than 2 microns. figure 2 For the synthesis product ...

Embodiment 2

[0027] Mix 0.5 mole of iron powder, 0.5 mole of ammonium dihydrogen phosphate, 0.55 mole of lithium hydroxide, and glucose accounting for 5% of the total weight of raw materials and put them into a rod mill jar, use water as the medium, and fully mix them on a rod mill Dry at 120°C for 12 hours. The dried mixture is mechanically stirred and granulated with a polyacrylamide solution of 10% by weight relative to the total weight of the raw materials. After granulation, it is placed in a shaft furnace under an argon atmosphere of 10 liters / min. , heated up to 350°C at a rate of 10°C / min for 20 hours, then synthesized at 700°C for 24 hours, and lowered to room temperature to obtain lithium iron phosphate. The measured tap density of lithium iron phosphate is 1.38g / cm 3 , the electrode sheet was also prepared according to the method of Example 1, and after being assembled into a battery, it was charged and discharged at a rate of 0.1C, and the measured reversible capacity was 153mA...

Embodiment 3

[0029]Mix 0.5 mole of iron powder, 0.26 mole of lithium carbonate, 0.5 mole of diammonium hydrogen phosphate, and polyethylene accounting for 20% of the total weight of the raw materials and put them into a rod mill tank, using ethanol as the medium, and fully mix them on a rod mill 5 hours, dry at 80 ℃, the mixture after drying is mechanically agitated and granulated with castor oil solution relative to the total weight of the raw material 3wt%, after granulation, the mixture is put into a shaft furnace, under 10 liters / min of argon Under an air atmosphere, the temperature was raised to 400°C at a rate of 10°C / min for 15 hours, then synthesized at 750°C for 24 hours, and then lowered to room temperature to obtain lithium iron phosphate. The measured tap density of lithium iron phosphate is 1.41g / cm 3 According to the method of Example 1, electrode sheets were prepared, assembled into a test battery, charged and discharged at a rate of 0.1C, and the reversible capacity was 155...

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Abstract

The invention relates to a preparation method of lithium iron phosphate as cathode material of lithium ion battery.The preparation method comprises the following steps: preparing iron powder, lithium compound and phosphorus compound according to the atomic ratio as follows: Li:Fe:P=(0.95-1.1):1:1; adding carbon or the precursor of carbon, mixing the mixture evenly in medium for 1-20 h, drying, pelleting, treating the obtained product at 300-500 DEG C for 1-20h in an inert atmosphere and synthesizing at 600-850 DEG C for 5-36h to obtain the lithium iron phosphate as cathode material. In the invention, the cheap iron power is used as a raw material, the carbon or the precursor of carbon is added and the mechanical granulating method is adopted so that the tap density and the conductivity oflithium iron phosphate are increased and the produced cathode material has the advantages of high specific capacity, good cycle performance and rate performance and the like. The preparation method of lithium iron phosphate has the advantages of simple preparation process, strong operability and easy realization of large-scale production.

Description

technical field [0001] The invention relates to a lithium iron phosphate (LiFePO 4 ) preparation method, which belongs to the technical field of lithium ion battery cathode material preparation. Background technique [0002] Since Japan's Sony Corporation developed lithium-ion batteries in 1990, the research and development of positive electrode materials has attracted people's attention. At present, the positive electrode materials used in commercialized lithium-ion batteries are mainly lithium-intercalated transition metal oxides, including lithium cobaltate, lithium nickelate, lithium manganate, etc. Among them, the most widely used lithium cobalt oxide material has been developed for its application in large-capacity batteries due to its shortcomings such as scarcity of resources, high price, and poor safety performance. Lithium manganese oxide materials with abundant resources and low raw material prices have low capacity and poor high-temperature cycle performance, w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/04
CPCY02E60/12Y02E60/10
Inventor 卢世刚金维华蔡振平张向军阚素荣
Owner CHINA AUTOMOTIVE BATTERY RES INST CO LTD