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Hydrothermal synthesis method for preparing iron phosphate lithium as anode material of lithium ion battery

A lithium-ion battery, lithium iron phosphate technology, applied in battery electrodes, circuits, electrical components, etc., can solve the problems of low bulk density, low volume specific capacity, low specific capacity, etc., and achieve easy control of process parameters and excellent battery performance. , the effect of uniform particle distribution

Inactive Publication Date: 2010-06-30
孙琦
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to two disadvantages of lithium iron phosphate: one is low electrical conductivity, resulting in poor high-rate charge and discharge performance and low actual specific capacity; the other is low bulk density, resulting in low volume specific capacity
These two shortcomings hinder the application of modified materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] 1. Configure iron source and phosphorus source aqueous solution, wherein the concentration of iron is 0.1-2 mol / liter, the concentration of phosphorus is phosphorus: iron=(1.0-1.5): 1, configure lithium source solution, the concentration is lithium: iron=3 : 1.

[0016] 3. Mix the above-mentioned iron source solution and phosphorus source solution, transfer to an autoclave, and stir for 10 minutes.

[0017] 4. Slowly add the prepared lithium source solution into the mixed solution in the autoclave and stir.

[0018] 5. Add 15%-30% reducing agent in mass ratio to the mixed liquid, adjust the pH value between 5.0-8.0 with acetic acid, and stir for 1-2 hours.

[0019] 6. Seal the autoclave, heat up to 180°C-200°C, and keep warm for 8-12h. Cool naturally to room temperature.

[0020] 7. Wash the obtained product 5-10 times with distilled water, disperse it with ethanol, and dry it in a drying oven at 70°C-90°C.

[0021] In the above preparation method 1, the iron source...

Embodiment 2

[0026] Prepare an aqueous solution of 0.3M lithium hydroxide, 0.1M diammonium hydrogen phosphate, and 0.1M ferrous oxalate, and weigh 10g of sucrose. Transfer ferrous oxalate and ammonium dihydrogen phosphate solution into the autoclave and stir with a stirrer for 10 minutes. Add the lithium hydroxide solution into the autoclave, add sucrose, continue stirring for 1 hour, adjust the pH to 5.0-8.0 with acetic acid, and seal the autoclave. Raise the temperature to 180°C and keep it warm for 8h. Then the reaction kettle is naturally cooled to room temperature, the obtained product is washed 5-10 times with distilled water, dispersed with ethanol, and dried in a drying oven at 70°C. The obtained lithium iron phosphate product was tested by SEM and electrical performance test, and the SEM showed that the particle size was about 3 μm, and the particle distribution was uniform. The tap density of the measured product is 2.0g / cm3. Using a lithium sheet as the negative electrode, th...

Embodiment 3

[0028] Prepare an aqueous solution of 0.45M lithium hydroxide, 0.15M diammonium hydrogen phosphate, and 0.15M ferrous oxalate, and weigh 20g of sucrose. Transfer the solution of ferrous oxalate and ammonium dihydrogen phosphate into the autoclave, and stir with a stirrer for 10 minutes. Add the lithium hydroxide solution into the autoclave, add ascorbic acid, continue stirring for 1.5 hours, adjust the pH to 5.0-8.0 with acetic acid, and seal the autoclave. Raise the temperature to 200°C and keep it warm for 8h. Then the reaction kettle is naturally cooled to room temperature, the obtained product is washed 5-10 times with distilled water, dispersed with ethanol, and dried in a drying oven at 80°C. The obtained lithium iron phosphate product was tested by SEM and electrical performance test, and the SEM showed that the particle size was about 4 μm, and the particle distribution was uniform. The tap density of the measured product is 2.4g / cm3. Using a lithium sheet as the ne...

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Abstract

The invention relates to a hydrothermal synthesis method for preparing iron phosphate lithium as an anode material of lithium ion battery, which belongs to the technical field of new energy materials. The hydrothermal synthesis method comprises the following steps of: mixing an iron source with phosphate, adding a lithium source, and after uniform agitation, putting the mixture into a high-pressure reaction kettle; then, adding a reducing agent, and maintaining the temperature at 180-200 DEG C for 8-12 h to produce spherical iron phosphate lithium, wherein the mol ratio of the lithium source to the iron source to the phosphate is 3:1:1. The invention provides a simple and one-step method for directly preparing iron phosphate lithium. The technological parameters of the method used for preparation are easily controlled; compared with a process using ferric iron as a raw material, the resource of ferrous iron as the raw material is wider; the prepared iron phosphate lithium powder particles have small mean particle diameter which is about 3-5 mu m, the particles are evenly distributed, the tap density can reach 2.0-2.5 g / cm<3>, the battery performance is high, and the specific capacity for the first charge and discharge cycle is 140-160 mAh / g.

Description

technical field [0001] The invention relates to a hydrothermal synthesis method for preparing lithium iron phosphate, an anode material of a lithium ion battery, and belongs to the technical field of new energy materials. Background technique [0002] Lithium-ion battery is a new generation of green high-energy battery, and is considered to be a high-tech product of great significance in the 21st century. It has many advantages such as high voltage, small self-discharge, high energy density, good cycle performance, no memory effect, wide working temperature range, etc. It is used in electronic instruments, various portable electric tools, mobile phones and other fields, especially in electric vehicles. It has a good application prospect in terms of application. The cathode material of lithium-ion batteries is an important part of lithium-ion batteries. At present, lithium cobalt oxide, lithium nickel oxide and lithium manganese oxide are more researched. Lithium cobalt oxi...

Claims

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Application Information

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IPC IPC(8): H01M4/1397H01M4/58
CPCY02E60/12Y02E60/122Y02E60/10
Inventor 孙琦朱小奕胡章勇
Owner 孙琦
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