Low-temperature hydro-thermal synthesis for nano-lithium iron phosphate

A lithium iron phosphate, hydrothermal synthesis technology, applied in the direction of phosphorus compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of poor performance consistency, long preparation time, complex process, etc., to achieve good application value, material particles The effect of uniform degree and easy process control

Inactive Publication Date: 2008-10-08
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These materials generally adopt solid-phase method and sol-gel method, which have disadvantages such as complicated process, long preparation time, high cost and poor performance consistency.

Method used

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  • Low-temperature hydro-thermal synthesis for nano-lithium iron phosphate
  • Low-temperature hydro-thermal synthesis for nano-lithium iron phosphate
  • Low-temperature hydro-thermal synthesis for nano-lithium iron phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 27.8g FeSO 4 ·7H 2 O and 13.2g (NH 4 ) 2 HPO 4 Dissolve in aqueous solution and mix well, add 18.6g disodium edetate (complexing agent), then add 6.04g LiCl·H 2 O. Place the precursor solution in an ultrasonic oscillator and vibrate for 5 minutes, then transfer it into a 100mL stainless steel autoclave lined with a polytetrafluoroethylene tank, fill the solution with a volume of 90%, add 6 grams of urea, seal the autoclave, and keep it warm at 150°C for 10 hours Afterwards, the furnace was cooled, and the reaction product was taken out.

[0028] The above reaction product was washed with ethanol, then washed with distilled water, and centrifuged with a high-speed centrifuge (10 min each time, rotating speed 8000 rpm), repeated 3 times. The obtained solid was dried in a vacuum oven at a temperature of 60° C. for 4 hours. After drying, place it in a tube furnace with nitrogen protection, raise the temperature to 400°C at a heating rate of 5°C / min, and cool naturall...

Embodiment 2

[0030] 39.2g (NH 4 )2Fe(SO 4 ) 2 ·6H 2 O and 11.53g of phosphoric acid were dissolved in the aqueous solution and mixed uniformly, after adding 18.6g of disodium edetate (complexing agent), 7.4g of Li 2 CO 3 ·H 2 O. Place the precursor solution in an ultrasonic oscillator and vibrate for 5 minutes, then transfer it into a 100mL stainless steel autoclave lined with a polytetrafluoroethylene tank, fill the solution with a volume of 90%, add 9 grams of urea, seal the autoclave, and keep it warm at 170°C for 10 hours Afterwards, the furnace was cooled, and the reaction product was taken out.

[0031] The above reaction product was washed with ethanol, then washed with distilled water, and centrifuged with a high-speed centrifuge (10 min each time, rotating speed 8000 rpm), repeated 3 times. The obtained solid was dried in a vacuum oven at a temperature of 60° C. for 4 hours. After drying, place it in a tube furnace with nitrogen protection, raise the temperature to 400 deg...

Embodiment 3

[0033] 27.8g FeSO 4 ·7H 2 O and 11.53g of phosphoric acid with a concentration of 85% were dissolved in an aqueous solution and mixed uniformly. After adding 18.6g of disodium edetate (complexing agent), 6.04g of LiCl·H was added under constant stirring. 2 O. Place the precursor solution in an ultrasonic oscillator and vibrate for 5 minutes, then transfer it into a 100mL stainless steel autoclave lined with a polytetrafluoroethylene tank, fill the solution with a volume of 90%, add 9 grams of urea, seal the autoclave, and keep it warm at 170°C for 10 hours Afterwards, the furnace was cooled, and the reaction product was taken out.

[0034] The above reaction product was washed with ethanol, then washed with distilled water, and centrifuged with a high-speed centrifuge (10 min each time, rotating speed 8000 rpm), repeated 3 times. The obtained solid was dried in a vacuum oven at a temperature of 60° C. for 4 hours. After drying, place it in a tube furnace with nitrogen prot...

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Abstract

The invention relates to a low temperature hydrothermal synthesis method for nano lithium ferrous iron phosphate and pertains to the technical field of production process of inorganic compound energy materials. In the method, aqueous solutions of ferrous salt and aqueous solutions of phosphate are mixed, proper amount of complexing agent is added, water-soluble lithium salt or lithium salt which is soluble in a weak acid environment is added, the ratio of lithium ion, ferrous ion and phosphate ion is 1-2:1:1 and the total concentration of the reaction system is 0.1-3.0mol / L; proper amount of pH regulator is added, resultant obtained after heating reaction in a high pressure reaction kettle is carried out washing, separating, drying and heat treatment to obtain nano lithium ferrous iron phosphate material. The method of the invention has simply controllable process, high yield of materials, no heavy metal pollution during the process, even particle of the materials and excellent electrochemical performance, which can be applied to electrode material of lithium-ion battery.

Description

technical field [0001] The present invention relates to a kind of nano iron ferrous phosphate (LiFePO 4 The low-temperature hydrothermal synthesis method of ) compound belongs to the technical field of nano inorganic compound energy material manufacturing technology. Background technique [0002] Due to the advantages of high voltage, high energy density, good cycle performance, small self-discharge, and no memory effect, lithium-ion batteries can meet the requirements of light, thin, and small portable electronic products, and become the most competitive supporting products in the above fields. After several years of market competition, lithium-ion batteries have occupied a dominant position in the field of mobile electronic terminal equipment such as notebook computers, mobile phones, and camcorders due to their excellent cost-effective advantages. At the same time, the application of lithium-ion batteries in vehicle batteries, uninterruptible power supplies, and large-sc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45H01M4/58
CPCY02E60/10
Inventor 赵兵焦正吴明红阎婧施文彦王松晏秀妹庄华陶海华仲明阳
Owner SHANGHAI UNIV
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