Microwave-hydrothermal method for preparing cathode materials of nano lithium iron phosphate batteries

A lithium iron phosphate battery and cathode material technology, applied in the microwave-hydrothermal field, can solve the problems of high energy consumption, complicated process, and large product particles

Inactive Publication Date: 2012-07-04
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the solid-phase method is carried out at a high temperature of 550-700 ° C and an inert gas condition, which has a long production cycle, high energy consumption, and the product has large particles, uneven distribution, and difficult to control the shape.
Commonly used liquid methods include hydrothermal method, co-precipitation method, sol-gel method, etc. Although the product is more pure than the solid-phase method, the particle size can reach nanoscale, and the shape controllability is improved, but there are also complex processes. Disadvantages of high cost, long cycle and harsh preparation conditions

Method used

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  • Microwave-hydrothermal method for preparing cathode materials of nano lithium iron phosphate batteries
  • Microwave-hydrothermal method for preparing cathode materials of nano lithium iron phosphate batteries
  • Microwave-hydrothermal method for preparing cathode materials of nano lithium iron phosphate batteries

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Weigh 0.333g of lithium hydroxide powder, dissolve it in deionized water, and prepare a 0.2g / mL lithium hydroxide aqueous solution. Weigh 0.736g of ferrous sulfate powder, dissolve it in a mixed solvent of deionized water and ethanol, add dropwise 0.15mL of phosphoric acid (85%), and stir magnetically for 5 minutes at a speed of 500 rpm to form a transparent mixed solution. Lithium hydroxide aqueous solution was added to this mixed solution to form a gray-green cloudy solution. Weigh 0.078g of ascorbic acid and 0.121g of hexadecyltrimethylammonium bromide respectively, add them into the turbid solution, stir magnetically for 10 minutes at a speed of 500 rpm, and measure the pH to be 5.8. Then, with a pressure of 1.5 MPa, the mixture was put into a quartz reaction tube, placed on a microwave reactor, heated to 150° C. by microwave, and kept at a constant temperature for 20 minutes. After the reaction, after centrifugation, ultrasonic cleaning, and vacuum heating and dry...

Embodiment 2

[0022] Weigh 0.333g of lithium hydroxide powder, dissolve it in deionized water, add dropwise 0.14mL of phosphoric acid (85%), and magnetically stir for 5 minutes at a speed of 500 rpm to form a white turbid solution. Weigh 0.736g of ferrous sulfate and 0.078g of ascorbic acid powder respectively, dissolve them in deionized water together, then add them to the white turbid liquid, stir magnetically for 10 minutes at a speed of 500 rpm, and form a gray-green turbid liquid. Measure the pH value of 6.0. Then, the gray-green turbid liquid was put into a quartz reaction tube, placed on a microwave reactor, heated to 150° C. by microwave, kept at a constant temperature for 20 minutes, and the pressure was 1.4 MPa. After the reaction, after centrifugation, ultrasonic cleaning and heating and drying, off-white loose nano-lithium iron phosphate powder is finally obtained, the microscopic appearance is nearly spherical particles, and the size is about 2.0nm.

Embodiment 3

[0024] Weigh 0.250g of lithium hydroxide powder, dissolve it in deionized water, add dropwise 0.11mL of phosphoric acid (85%), and magnetically stir for 5 minutes at a speed of 500 rpm to form a white turbid solution. Weigh 0.524g of ferrous sulfate and 0.017g of calcium acetate powder, dissolve them together in deionized water, add them to the white turbid solution, and stir magnetically for 10 minutes at a speed of 500 rpm to form a gray-green turbid solution. Weigh 0.182g of cetyltrimethylammonium bromide, add it into the turbid liquid and mix evenly, and measure the pH value to be 6.0. Then, the mixed turbid solution was put into a quartz reaction tube, placed on a microwave reactor, heated to 150° C. by microwave, kept at a constant temperature for 20 minutes, and the pressure was 1.1 MPa. After the reaction, after centrifugation, ultrasonic cleaning and heating and drying, off-white loose nano-lithium iron phosphate powder is finally obtained.

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Abstract

The invention provides a microwave-hydrothermal method for preparing cathode materials of nano lithium iron phosphate batteries, which includes the following steps that water-soluble lithium source compounds, iron source compounds and phosphorus source compounds serve as main reactants and are added with reaction additives, and are arranged in a microwave reaction instrument to have a microwave-hydrothermal reaction after being uniformly fixed in water or mixed solvent of water and other solvent, thereby obtaining ideal cathode materials of the nano lithium iron phosphate batteries under mild conditions (the temperature is 100-250 DEG C and the intensity of pressure is 0.1-1.5MPa ). The microwave-hydrothermal method for preparing cathode materials of nano lithium iron phosphate batteries has the advantages of being simple in process, energy-saving, high in efficiency, mild in conditions, low in cost, excellent in purity of products, uniform and fine in particles, high in controllability and excellent in reproducibility.

Description

technical field [0001] The invention relates to a microwave-hydrothermal method for preparing anode materials of nanometer lithium iron phosphate batteries, belonging to the technical field of cathode materials for lithium ion batteries. Background technique [0002] Modern life advocates low-carbon life and green consumption. In 2009, my country became the second largest carbon dioxide emitter in the world. The task of energy conservation and emission reduction is extremely arduous, and the dependence on foreign crude oil imports exceeded 50% for the first time. The new energy industry has become one of the key areas that China and other countries focus on. Battery research and development has become the center of competition for the new energy industry. [0003] As a new type of power source, lithium-ion batteries have become the first choice for power battery research and development due to their advantages such as light weight, large capacity, no memory effect, non-toxic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45
Inventor 卢灿忠常金晶
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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