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Method for preparing high-power lithium iron phosphate composite materials

A technology of lithium iron phosphate and composite materials, applied in phosphorus compounds, chemical instruments and methods, electrode manufacturing, etc., can solve problems such as restricting the application range of lithium iron phosphate batteries, decrease in battery energy density, heat generation, etc., and achieve large-scale industrialization. Production, excellent electrochemical performance, the effect of reducing the reaction barrier

Inactive Publication Date: 2010-01-06
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the field of electric tools, due to the high requirements on the discharge rate, it is generally required to continue to discharge at 10C, while the particles prepared by the traditional solid-state reaction method are relatively large (the average size of the primary particles is about 0.5um), and the electronic conductivity and ion diffusivity are relatively large. Poor reasons have restricted the application range of lithium iron phosphate batteries
Currently commercially available batteries made of lithium iron phosphate materials have two significant defects at high currents: one is that the voltage is reduced due to the polarization effect of discharge at a higher rate, and the average voltage after discharge at 10C generally does not exceed 2.85V, in this way, the energy density of the battery has dropped by more than 10% compared with the conventional one; the second is that during the high-rate discharge period, severe heating occurs. When discharging at 20C, the temperature reaches about 70 degrees. Due to the phenomenon of iron ion dissolution at high temperature, it has an adverse effect on the cycle life and safety of the battery.

Method used

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  • Method for preparing high-power lithium iron phosphate composite materials
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  • Method for preparing high-power lithium iron phosphate composite materials

Examples

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Embodiment 1

[0018] Example 1. Under room temperature, 27g ferric nitrate Fe(NO3) 3.9H2O and 200ml concentrated nitric acid are uniformly mixed under the rotating speed of 600 revs / min, then add 0.5g carbon nanotube, ultrasonic dispersion, reflux 4.5 hours in the oil bath of 120 degree, will The temperature of the refluxed mixture is lowered to 20 degrees, and the pH value is adjusted to 10 with 3.0wt% ammonia solution and 50g of 3.2wt% lithium hydroxide solution, and stabilized for 5 minutes to obtain a suspension of iron hydroxide precursor embedded with carbon nanotubes liquid. Then slowly add 18ml of 1.5mol / L phosphoric acid and 20ml of 2.0mol / L diammonium hydrogen phosphate dropwise, stirring while adding dropwise; after the dropwise addition is completed, stop stirring. The reaction system was distilled under reduced pressure to obtain a lithium iron phosphate precursor embedded with carbon nanotubes. Grind the precursor powder and place it in a tube furnace, use 80% nitrogen and 2...

Embodiment 2

[0019] Example 2. At room temperature, 13.5g of ferric nitrate Fe(NO3)3.9H2O and 5.41g of ferric chloride FeCl3 were uniformly mixed with 200ml of concentrated nitric acid at a speed of 550 rpm, then 0.8g of carbon nanotubes were added, ultrasonically dispersed, and heated at 120 degrees Reflux in an oil bath for 4.5 hours, reduce the temperature of the refluxed mixture to 20 degrees, add 100 g of 2.48% lithium carbonate suspension, then adjust the pH value of the reaction solution to 9 with 4.0% wt of ammonia solution, and stabilize it for 5 minutes to obtain The ferric hydroxide precursor suspension embedded with carbon nanotubes; then slowly add 18ml of 1mol / L phosphoric acid and 49ml of 1mol / L diammonium hydrogen phosphate dropwise, stirring while adding; after the dropwise addition, stop stirring. The reaction system was distilled under reduced pressure to obtain a lithium iron phosphate precursor embedded with carbon nanotubes. Grind the precursor powder and place it in...

Embodiment 3

[0020] Example 3. Under room temperature, 36g ferric nitrate Fe(NO3) 3.9H2O and 200ml concentrated nitric acid are uniformly mixed under the rotating speed of 600 rpm, then add 0.8g carbon nanotube, ultrasonic dispersion, reflux 5 hours in the oil bath of 120 degree, will The temperature of the refluxed mixture was lowered to 25 degrees, and 100 g of a suspension solution containing 1.65 wt % lithium carbonate and 2.28 wt % lithium acetate was added, and then the pH value of the reaction solution was adjusted to 9 with 3.5 wt % ammonia water, and stabilized for 5 min to obtain Iron hydroxide precursor suspension embedded with carbon nanotubes; then slowly add 24ml of 1mol / L phosphoric acid and 65ml of 1mol / L diammonium hydrogen phosphate dropwise, and stir while adding; after the dropwise addition, stop stirring. The reaction system was distilled under reduced pressure to obtain a lithium iron phosphate precursor embedded with carbon nanotubes. Grind the precursor powder and ...

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Abstract

The invention relates to a method for preparing high-power lithium iron phosphate composite materials, which belongs to the technical field of the preparation of lithium battery materials. The invention aims to provide the method for preparing the high-power lithium iron phosphate composite materials which can solve the problem that lithium iron phosphate has low electronic conductivity and difficult ion diffusion in high rate discharge. The invention is technically characterized by making carbon nanotubes reflux in concentrated nitric acid containing iron salt, adding ammonia water and hydroxide ions in a lithium source into the concentrated nitric acid to react to obtain iron hydroxide suspension solution embedded with the carbon nanotubes; then adding phosphate solution into the iron hydroxide suspension solution to obtain iron phosphate suspension solution embedded with the carbon nanotubes; and performing distillation on the iron phosphate suspension solution under reduced pressure to obtain a precursor of the lithium iron phosphate, and grinding the precursor and performing high-temperature sintering in a reductive and inert atmosphere to obtain the high-conductivity lithium iron phosphate composite materials. The lithium iron phosphate composite materials have good shapes with an average grain diameter of 10 to 100nm and excellent electrochemical performance, are particularly suitable for ultrahigh rate discharge requirement, and can meet the requirement of sustained 30C discharge and pulse 100C discharge.

Description

technical field [0001] The invention relates to a preparation method of a high-power lithium iron phosphate composite material, belonging to the technical field of lithium battery material preparation. Background technique [0002] Lithium iron phosphate has become the preferred cathode material for lithium power batteries because of its excellent safety performance and excellent cycle performance. In addition, lithium iron phosphate is also widely used in UPS power supply systems of mobile phones, notebook computers, digital cameras and a large number of other emerging IT products. At present, lithium iron phosphate batteries have begun to substantially replace traditional lead-acid batteries in large-scale power batteries such as electric vehicles, electric tools, automotive 42V batteries, and photovoltaic energy storage batteries. [0003] In the field of electric tools, due to the high requirements on the discharge rate, it is generally required to continue to discharge...

Claims

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Application Information

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IPC IPC(8): H01M4/04H01M4/58H01M4/48C01B25/45B01J19/00
CPCY02E60/12Y02E60/10
Inventor 蒋华锋徐小明
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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