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Preparation method of hollow ferric oxide cathode material in porous structure

A technology of porous structure and negative electrode material, applied in the direction of iron oxide, iron oxide/iron hydroxide, structural parts, etc., can solve the problems of low theoretical electrochemical capacity, unsatisfactory first discharge efficiency, poor cycle performance, etc., and achieve a simple process. Controllable, beneficial to material rate and cycle performance, and the effect of uniformity assurance

Inactive Publication Date: 2018-01-12
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the anodes of commercial lithium-ion batteries are generally carbon materials such as graphite and carbon fiber, but their relatively low theoretical electrochemical capacity, unsatisfactory initial discharge efficiency, and poor cycle performance make it urgent to seek new anode materials to replace carbon materials.

Method used

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  • Preparation method of hollow ferric oxide cathode material in porous structure
  • Preparation method of hollow ferric oxide cathode material in porous structure
  • Preparation method of hollow ferric oxide cathode material in porous structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh 0.1g of potassium ferricyanide and 0.05g of 1,3,5-benzenetricarboxylic acid, put them into a 100mL polytetrafluoroethylene reaction kettle, add 80ml of absolute ethanol, stir well, and adjust the pH value of the solution with 1mol / L hydrogen chloride to 5. After sealing the reaction kettle, keep it warm at 200° C. for 10 h, cool down to room temperature with the furnace, filter the reaction product, wash it 4 times with deionized water, and dry it. Put the dried product into a tube furnace, heat up at a rate of 1°C / min in an air atmosphere, heat at 800°C for 1 hour, and then cool down with the furnace to obtain a hollow cubic iron oxide material. The XRD test shows that the obtained material has high diffraction intensity and is a pure-phase iron oxide negative electrode material, such as figure 1 shown. It can be seen from the scanning electron microscope that the particle size of iron oxide is uniform and the hollow porous structure, such as figure 2 shown. ...

Embodiment 2

[0026] Weigh 0.15g of ferric nitrate and 0.06g of trimesic acid, put them into a 100mL polytetrafluoroethylene reactor, add a mixed solution of 70ml of methanol and 10ml of water, stir evenly, and use 1mol / L ammonia water to adjust the pH value of the solution to 9 . After sealing the reaction kettle, keep it warm at 100°C for 72 hours, cool down to room temperature with the furnace, filter the reaction product, wash it three times with deionized water, and dry it. Put the dried product into a tube furnace, heat up at a rate of 5°C / min in an air atmosphere, heat at 600°C for 2 hours, and then cool with the furnace to obtain a porous iron oxide negative electrode material.

Embodiment 3

[0028] Weigh 0.5 g of ferric sulfate and 0.09 g of 4-pyridinecarboxylic acid, put them into a 100 ml polytetrafluoroethylene reactor, add 80 ml of absolute ethanol, stir well, and adjust the pH value of the solution to 10 with 2 mol / L triethylamine. After sealing the reaction kettle, keep it warm at 130° C. for 10 h, cool down to room temperature with the furnace, filter the reaction product, wash it 4 times with deionized water, and dry it. Put the dried product into a tube furnace, heat up at a rate of 4°C / min in an air atmosphere, heat at 200°C for 0.5h, and then cool with the furnace to obtain an iron oxide negative electrode material.

[0029] image 3 It is the rate performance graph of the iron oxide negative electrode material prepared in Example 3 of the present invention. The electrochemical test results show that compared with the conventional solid-phase method and liquid-phase method, the rate performance of the material is greatly improved. The specific discharg...

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Abstract

The invention discloses a preparation method of a hollow iron oxide cathode material in a porous structure. The preparation method comprises the steps of weighing an organic ligand compound and iron salt at a mole ratio of 1:(1-10), adding a solvent, performing uniform stirring and dispersion, allowing a mass ratio of a solute to the solvent to be 1:(100-800), preparing a high polymer coordinationpolymer by a hydrothermal / solvothermal method under conditions of a pH (potential of hydrogen) value of 3-11, the temperature of 100-200 DEG C and reaction time of 10-72h, roasting the prepared polymer at a 200-800 DEG C oxygen-containing atmosphere, and obtaining the hollow iron oxide cathode material in a multilevel structure. A hollow ferric oxide particle in the porous structure is obtained by a hydrothermal / solvothermal - high-temperature burning two-step method; the method has the advantages that ferric ions are arrayed orderly in a long range in a lattice; an organic framework supporting the ferric ion can limit growth of the ferric oxide particle in a three-dimensional direction via aerobic burning; the obtained ferric oxide particle is good in particle size uniformity and dispersity; and the increase and improvement of a multiplying factor and cycle performance of a material are facilitated.

Description

technical field [0001] The invention belongs to the field of preparation of lithium-ion secondary battery materials, in particular to a method for preparing a hollow porous structure iron oxide negative electrode material. Background technique [0002] In recent years, lithium-ion secondary batteries have developed rapidly, and their obvious advantages such as high voltage, high energy density, low self-discharge rate, and high cycle life make lithium-ion secondary batteries are playing an increasingly important role. It is precisely because lithium-ion secondary batteries are more and more widely used that people have higher and higher requirements for their performance, including energy density, cycle life and safety performance of batteries. Material improvements. At present, the anodes of commercial lithium-ion batteries are generally carbon materials such as graphite and carbon fiber, but their relatively low theoretical electrochemical capacity, unsatisfactory initia...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/06H01M4/525H01M10/0525
CPCY02E60/10
Inventor 许鹏
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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