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Method for synthesizing lithium iron phosphate and carbon nanotube composite material in situ

A technology of lithium iron phosphate and carbon nanotubes, which is applied in the direction of electrical components, battery electrodes, circuits, etc., can solve the problems of high price and high cost, and achieve the effects of uniform distribution, flat discharge platform, and lower volume resistivity

Inactive Publication Date: 2012-07-04
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, carbon nanotubes in the market are mainly produced by the arc discharge method, and the price is generally high. 4 The cost of carbon nanotubes coated with finished products is too high, resulting in many LiFePO 4 Manufacturers stay away

Method used

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  • Method for synthesizing lithium iron phosphate and carbon nanotube composite material in situ
  • Method for synthesizing lithium iron phosphate and carbon nanotube composite material in situ
  • Method for synthesizing lithium iron phosphate and carbon nanotube composite material in situ

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] a) Weigh 98.4g Fe-- -- PO-- 4 , 25.4gLi 2 CO 3 , 15.4g of glucose, 0.37g of ferrocene were milled for 3h in a ball mill jar with alcohol as the milling medium;

[0021] b) Pump the stirred mixed slurry into a clean container, place it in a drying oven, and control the temperature of the drying oven to 70°C. After the alcohol is completely evaporated, the obtained solid powder is milled with a ball mill jar for 2 hours;

[0022] c) The dry material after ball milling is kept at 180°C for 1 hour in a nitrogen atmosphere, then heated to 400°C and held for 2.5 hours, then the nitrogen flow is replaced by a mixed flow of nitrogen and benzene steam, and the flow rate of the stupid steam is controlled at 2.5ml / min Afterwards, the temperature was raised to 820° C. for sintering for 9 hours to obtain a composite material of carbon nanotubes and lithium iron phosphate. The 0.2C discharge capacity is 162mAh / g, and the 2C discharge capacity is 150mAh / g.

Embodiment 2

[0024] a) Weigh 54.7g FeC 2 o 2 2H 2 O, 11.7gLi 2 CO 3 , 34.51gNH 4 ·H 2 PO 4 , 7.2g sucrose and 0.17g ferrocene were milled in a ball mill tank with alcohol as the milling medium for 4h;

[0025] b) Pump the stirred mixed slurry into a clean container, place it in a drying oven, and control the temperature of the drying oven to 70°C. After the alcohol is completely evaporated, the obtained solid powder is milled with a ball mill jar for 2 hours;

[0026] c) The dry material after ball milling is kept at 200°C for 1.5h in a nitrogen atmosphere, then heated up to 420°C and held for 2h, then the nitrogen flow is replaced by a mixed flow of nitrogen and benzene steam, and the flow of stupid steam is controlled at 15ml / min. , the temperature was programmed to 830° C. for sintering for 11 hours, and the composite material of carbon nanotubes and lithium iron phosphate was obtained.

Embodiment 3

[0028] a) Weigh 54.7g FeC 2 o 2 2H 2 O, 7.2gLiOH, 34.1gNH 4 ·H 2 PO 4 , 7.53g of maleic acid and 0.16g of ferrocene were milled for 4h in a ball milling tank with acetone as the milling medium;

[0029] b) Pump the mixed slurry after ball milling into a clean container, place it in a drying oven, and control the temperature of the drying oven to 70°C. After the alcohol is completely evaporated, the obtained solid powder is milled with a ball mill jar for 2.5 hours;

[0030] c) The dry material after ball milling is kept at 200°C for 2 hours in a nitrogen atmosphere, then heated to 420°C and kept for 2 hours, then the nitrogen flow is replaced by a mixed flow of nitrogen and benzene steam, and the flow of toluene steam is controlled at 8ml / min. The temperature was programmed to rise to 840° C. for sintering for 11 hours to obtain a composite material of carbon nanotubes and lithium iron phosphate.

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Abstract

The invention discloses a method for synthesizing a lithium iron phosphate and carbon nanotube composite material in situ. The method comprises the following steps of: uniformly mixing an iron source, a lithium source, a carbon source, a phosphor source and a catalyst, i.e. dicyclopentadienyl iron in a stirring mill with alcohol as a medium; performing drying and ball milling on the mixture; and sintering the mixture in nitrogen gas and mixed aromatic hydrocarbon mixed gas for 4 to 20 hours at the temperature of 400 to 1,000 DEG C to obtain the composite material. While the lithium iron phosphate is generated, a carbon nanotube is grown on the surface of a particle in situ, and a conducting network is formed in a secondary coacervate. The method has the characteristics of simple process, low energy consumption and high efficiency. The prepared material is high in purity, relatively small in particle size and excellent in electrochemical performance. The synthesized lithium iron phosphate is relatively flat in discharge platform, wherein the discharge capacity of 0.2C lithium iron phosphate is 162mAh / g, and the discharge capacity of 2C lithium iron phosphate is 150mAh / g.

Description

technical field [0001] The invention belongs to the preparation of lithium ion battery cathode materials, in particular to a preparation method for in-situ synthesis of lithium iron phosphate and carbon nanotube composite materials. Background technique [0002] In this new era of advocating green and low-carbon economy, lithium-ion batteries are widely used in various fields due to their unique advantages such as high energy, high voltage, long life, low self-discharge, and no memory effect. Of which LiFePO 4 It has no volume change during lithium extraction and insertion, and does not release active oxygen during charging and discharging at high temperatures. It has excellent cycleability and safety, and has gradually become one of the most popular cathode materials for lithium-ion batteries. But it is undeniable that the pure phase of LiFePO 4 The electronic conductivity of the ions is extremely low, and the ion diffusion rate is also unsatisfactory. Therefore, how...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M4/1397
CPCY02E60/122Y02E60/10
Inventor 张龙
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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