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Hydrothermal synthesis preparation method of ion doping high-performance lithium iron phosphate

A lithium iron phosphate, ion doping technology, applied in electrical components, battery electrodes, circuits, etc., can solve the problems of unsatisfactory lithium ion diffusion rate, uneven particle distribution, poor high rate performance, etc., and achieve excellent electrochemical performance. , The process control is simple, the crystallinity is good

Inactive Publication Date: 2012-01-11
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the electronic conductivity of LiFePO4 is extremely low, only 10-7~10-9S / cm at room temperature, which belongs to a semiconductor material; moreover, the lithium ion diffusion rate of this material is not satisfactory, which makes it have a high capacity when charging and discharging with a large current. Rapid decline, poor high-rate performance, and LiFePO 4 In the preparation process, there are disadvantages such as complicated process, high energy consumption, high cost, poor performance consistency and uneven particle distribution, which restrict the LiFePO 4 practical application of

Method used

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  • Hydrothermal synthesis preparation method of ion doping high-performance lithium iron phosphate
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  • Hydrothermal synthesis preparation method of ion doping high-performance lithium iron phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] a): see Figure 1-Figure 3 , the 1021.65g FeSO 4 ·7H 2 O, 9.73gNiCl 2 , 100g of ascorbic acid and 432.5g of 85% H 3 PO 4 Mix together, add 5.925g of polyvinyl alcohol, then add 2.5L of deionized water, and then keep stirring,

[0023] At the same time, 472gLiOH·H 2 O (analytical pure) was dissolved in 2.5L of deionized water and stirred to obtain a lithium oxide solution, and then the lithium hydroxide solution was slowly added dropwise to the mixed solution to adjust the pH value to 8. Then the mixed solution was transferred to a 10L reaction kettle, deionized water was added appropriately, sealed, and kept at 180° C. for 2 hours.

[0024] b): After the above reaction is completed, cool to room temperature, filter and wash the product, and dry the filter cake in a vacuum at 80° C. for 12 hours to obtain nickel-containing lithium iron phosphate powder.

[0025] c): The nickel-containing lithium iron phosphate powder and maleic acid are ball-milled in an alcohol s...

Embodiment 2

[0027] a): 457.2g of FeCl 2 , 19.46gNiCl 2 , 98.8g of maleic acid and 432.5g of 85% H 3 PO 4 Mix together, add 8.89g of polyacrylamide, then add 2.5L of deionized water, and then keep stirring. At the same time, 742.5g of lithium acetate (analytical pure) was dissolved in 2.5L of deionized water, and stirred to obtain a pure solution. Then the lithium acetate solution was slowly added dropwise to the mixed solution to adjust the pH value to slightly alkaline. Then the mixed solution was transferred to a 10L reaction kettle, deionized water was added appropriately, sealed, and kept at 190° C. for 2 hours.

[0028] b): After the above reaction is completed, cool to room temperature, filter and wash the product, and dry the filter cake in a vacuum at 90° C. for 12 hours to obtain nickel-containing lithium iron phosphate powder.

[0029] c): The nickel-containing lithium iron phosphate powder and citric acid are ball-milled in an alcohol solution at a mass ratio of 10:3 for...

Embodiment 3

[0031] a): 409.93g of iron acetate, 8.84g of nickel acetate, 100g of ascorbic acid and 431.25 of NH 4 h 2 PO 4 Mix together, add a mixture of 11.85 polyvinyl alcohol and polyacrylamide, then add 2.5 L of deionized water, and then keep stirring. At the same time, 472gLiOH·H 2 O (analytically pure) was dissolved in 2.5L deionized water, stirred to obtain a pure solution, and then slowly added dropwise to the mixed solution to adjust the pH value to weakly alkaline. Then the mixed solution was transferred to a 10L reaction kettle, deionized water was added appropriately, sealed, and kept at 200°C for 1.5h.

[0032] b): After the above reaction is completed, cool to room temperature, filter and wash the product, and dry the filter cake in a vacuum at 95° C. for 12 hours to obtain nickel-containing lithium iron phosphate powder.

[0033] c): The nickel-containing lithium iron phosphate powder and citric acid are ball-milled in an alcohol solution at a mass ratio of 5:1 for 2 ...

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Abstract

The invention relates to a hydrothermal synthesis preparation method of ion doping high-performance lithium iron phosphate. Iron source, nickel source, organic acid and phosphorus source are dissolved in deionized water according to a certain proportion, added with a dispersing agent, and mixed to obtain a mixed solution; lithium source which is uniformly dissolved in deionized water is dropwise and slowly added into the mixed solution; a pH is adjusted to 7.5-8.2 after dropping; the obtained alkalescent mixed solution is transferred to an autoclave; the autoclave is enclosed and insulated at 80-220 DEG C for 1 h-3 h; after cooling the autoclave is opened, and products are taken out, filtered with deionized water for several times and washed; an obtained filter cake is dried; then the obtained nickelic lithium iron phosphate powder and carbon contained organic compound in a mass ratio of 10:1-4 are treated with ball-milling for 1-3 h in alcohol, dried and sintered for 1-4 h at 600-800 DEG C under protection of nitrogen to obtain the product.

Description

technical field [0001] The invention relates to the preparation of lithium-ion battery cathode materials, specifically a hydrothermal synthesis preparation method of ion-doped high-performance lithium iron phosphate. Background technique [0002] In the early 1990s, after the lithium-ion secondary battery was successfully developed by Japan's SONY company, it became a research hotspot all over the world. Compared with lead-acid batteries, nickel-cadmium batteries and nickel-hydrogen batteries, lithium-ion secondary batteries have the advantages of high working voltage, high specific energy, small size, no memory effect and long cycle life. At present, lithium-ion secondary batteries are widely used in portable electronic devices such as mobile phones, notebook computers and cameras; meanwhile, they also have considerable application prospects in fields such as electric vehicles, aviation, aerospace and space technology. The most widely used cathode material for lithium-ion...

Claims

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Application Information

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IPC IPC(8): H01M4/58
CPCY02E60/10
Inventor 曹贺坤陈海涛张羽
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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