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Hydrothermal synthesis method for preparing nano-scale carbon-coated lithium iron phosphate

A technology of carbon-coated lithium iron phosphate and hydrothermal synthesis, applied to electrical components, battery electrodes, circuits, etc., can solve the problems of poor ion conductivity of active materials, affecting high-rate discharge performance, slow migration and diffusion, etc. , to achieve the effects of easy industrial production, accelerated diffusion speed, and uniform particle distribution

Inactive Publication Date: 2011-05-25
JIANGSU DELI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The lithium iron phosphate synthesized by known methods has the following disadvantages: (1) ferrous iron Fe in the synthesis process 2+ Easily oxidized to ferric iron Fe 3+ , it is difficult to obtain pure-phase lithium iron phosphate, that is, there are many impurities, which affect the capacity; (2) the particles are coarse and uneven, and lithium ions in LiFePO 4 The speed of migration and diffusion in the medium is slow, which leads to poor ion conductivity of the active material and affects the charge and discharge speed; (3) LiFePO 4 The electrical conductor itself is low, which affects its high-rate discharge performance

Method used

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  • Hydrothermal synthesis method for preparing nano-scale carbon-coated lithium iron phosphate
  • Hydrothermal synthesis method for preparing nano-scale carbon-coated lithium iron phosphate
  • Hydrothermal synthesis method for preparing nano-scale carbon-coated lithium iron phosphate

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Embodiment 1

[0027] According to the molar ratio of Li:Fe:P=3:1:1, take 12.6 kg of lithium hydroxide monohydrate (LiOH·H 2 O) add 100 liters of deionized water, get 27.8 kilograms of ferrous sulfate heptahydrate (FeSO 4 ·7H 2 O) add 200 liters of deionized water, get 11.5 kilograms of phosphoric acid (85% H 3 PO 4 ) and 30 liters of deionized water were added to prepare aqueous solutions. Expected target product 15 kilograms. First, add phosphoric acid solution in the reaction kettle, then add ferrous sulfate solution, then add 1.5 kg of carbon black, after fully stirring and mixing, add lithium hydroxide solution, and finally add 350 liters of glycerin. Nitrogen was blown from the bottom of the reactor for one hour, all the air in the reactor was exhausted, and then the reactor was sealed and heated to 120°C for 3 hours. After cooling, the product was filtered, washed, vacuum-dried and dried. Finally, put it into a sagger, and sinter it through a mesh belt furnace. Sintering conditio...

Embodiment 2

[0030] According to the molar ratio of Li:Fe:P=1:1:1, take 6.9 kg of lithium nitrate (LiNO 3 ) plus 100 liters of deionized water, get 12.7 kg of ferrous chloride (FeCl 2 ) plus 200 liters of deionized water and 11.5 kg of phosphoric acid (85% H3 PO 4 ) and 30 liters of deionized water were added to prepare aqueous solutions. Expected target product 10 kilograms. Take 0.5kg of cetyltrimethylammonium bromide, add 2 liters of deionized water at about 35°C and stir thoroughly to prepare a dispersant solution. First, add phosphoric acid solution into the reaction kettle, then add ferrous chloride solution, then add 0.5 kg of sucrose and 0.5 kg of carbon black, after fully stirring and mixing, add lithium nitrate solution, along with adding dispersant solution, finally add 350 liters of poly ethylene glycol. Nitrogen was blown from the bottom of the reactor for one hour, all the air in the reactor was exhausted, and then the reactor was sealed and heated to 150°C for 3 hours. A...

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Abstract

The invention discloses a hydrothermal synthesis method for preparing nano-scale carbon-coated lithium iron phosphate, which belongs to the field of lithium-ion battery anode materials and comprises the following steps of: sequentially adding a phosphorus-source solution, an iron-source solution, a carbon source, a lithium-source solution and a boiling-point elevator into a reaction device in sequence, mixing, then heating to the temperature of 60-180 DEG C for reaction under inert gas, cooling after the reaction, filtering precipitates to obtain a nano-scale lithium iron phosphate precursor, and then sintering the nano-scale lithium iron phosphate precursor at the temperature of 400-600 DEG C under the protection of the mixed gas of the inert gas and hydrogen gas. The combination of lithium, iron, phosphorus and the like on a molecular level is realized by the method, and the grains of a product are quite fine and are uniformly distributed; because the boiling-point elevator is adopted, the reaction temperature and pressure of the reaction kettle are decreased; and the hydrothermal synthesis method has the advantages of simple preparation process, short flow, easiness in operational control, low reaction temperature, short time, low energy consumption and easiness in realizing large-scale industrialized production.

Description

technical field [0001] The invention belongs to the field of positive electrode materials of lithium ion batteries, and in particular relates to a preparation method of nanoscale carbon-coated lithium iron phosphate as the positive electrode material of lithium ion batteries. Background technique [0002] With the rapid development of new energy vehicles, lithium-ion batteries, especially lithium-ion batteries with lithium iron phosphate materials as the positive electrode, will be widely used in hybrid electric vehicles (HEV) and pure electric vehicles (EV). Compared with lithium-ion batteries of other cathode materials, lithium iron phosphate batteries have the advantages of long cycle life, good safety, fast charge and discharge, low cost, and no pollution. The lithium iron phosphate synthesized by known methods has the following disadvantages: (1) ferrous iron Fe in the synthesis process 2+ Easily oxidized to ferric iron Fe 3+ , it is difficult to obtain pure-phase lit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/1397
CPCY02E60/12Y02E60/122Y02E60/10
Inventor 朱跃中
Owner JIANGSU DELI CHEM
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