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Silicon oxide/carbon composite negative electrode material of lithium ion secondary battery and preparation method of silicon oxide/carbon composite negative electrode material

A technology for secondary batteries and negative electrode materials, applied in the field of silicon oxide/carbon composite negative electrode materials and their preparation, can solve problems such as poor cycle stability, and achieve the effects of long cycle life, increased specific surface area, and reduced oxygen participation

Inactive Publication Date: 2014-02-19
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The present invention is particularly aimed at the problem of poor cycle stability of silicon in the process of electrochemical lithium absorption and discharge, and provides a high-capacity, long-life lithium-ion secondary battery negative electrode material and a preparation method thereof

Method used

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  • Silicon oxide/carbon composite negative electrode material of lithium ion secondary battery and preparation method of silicon oxide/carbon composite negative electrode material
  • Silicon oxide/carbon composite negative electrode material of lithium ion secondary battery and preparation method of silicon oxide/carbon composite negative electrode material
  • Silicon oxide/carbon composite negative electrode material of lithium ion secondary battery and preparation method of silicon oxide/carbon composite negative electrode material

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Embodiment 1

[0024] 1) First, the precursor is prepared by the acid-base sol-gel method:

[0025] Glucose 2.48g was completely dissolved in water, and then 22.8ml of absolute ethanol was added. After stirring evenly by magnetic force, it was added to a 16.1% by volume ethyl orthosilicate ethanol solution. After mixing well, add 0.1 mol / L hydrochloric acid solution (the volume ratio of the added amount of hydrochloric acid solution to water is 1:10). After reacting at room temperature for 6 hours, 0.20ml of 0.1mol / L ammonia water was added dropwise until a stable gel was formed, aged at room temperature for 1 day, and dried at 70°C for 3 days to obtain a xerogel precursor.

[0026] 2) Secondly, the added carbon source and the original carbon source are mixed in a ball mill with a mass ratio of 1:1 for high-energy dry milling (the ball mill is a QM-3SP2 planetary ball mill produced by Nanjing University Instrument Factory, the same below), Wherein, the mass ratio of ball to material is 10:1...

Embodiment 2

[0035] 1) First, the precursor is prepared by the acid-base sol-gel method:

[0036]After 3.02 g of glucose was completely dissolved in water, 25.1 ml of absolute ethanol was added, and evenly stirred by magnetic force, then added to a 19.2% volume percent ethyl orthosilicate ethanol solution. After mixing well, add 0.1 mol / L hydrochloric acid solution (the volume ratio of the added amount of hydrochloric acid solution to water is 3:10). After reacting at room temperature for 10 hours, 0.24ml of 0.1mol / L ammonia water was added dropwise until a stable gel was formed, aged at room temperature for 2 days, and dried at 100°C for 2 days to obtain a xerogel precursor.

[0037] 2) Secondly, the added carbon source is mixed with the original carbon source by high-energy dry milling at a mass ratio of 1:1.2, wherein the mass ratio of balls to material is 5:1, and the dry gel precursor obtained above is ground , adding glucose and ball milling at 400 r / min for 6 h to obtain a precurso...

Embodiment 3

[0043] 1) First, the precursor is prepared by the acid-base sol-gel method:

[0044] 3.69 g of glucose was completely dissolved in water, and then 29.2 ml of absolute ethanol was added. After magnetically stirring evenly, it was added to a 24.4% volume percent ethyl orthosilicate ethanol solution. After mixing well, add 0.1 mol / L hydrochloric acid solution (the volume ratio of the added amount of hydrochloric acid solution to water is 5:10). After reacting at room temperature for 12 hours, 0.35ml of 0.1mol / L ammonia water was added dropwise until a stable gel was formed, aged at room temperature for 1 day, and dried at 80°C for 3 days to obtain a xerogel precursor.

[0045] 2) Secondly, the added carbon source is mixed with the original carbon source by high-energy dry milling at a mass ratio of 1:1.5, wherein the mass ratio of balls to material is 20:1, and the dry gel precursor obtained above is ground , adding glucose and ball milling at 500 rpm for 8 hours to obtain a pre...

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Abstract

The invention relates to a silicon oxide / carbon composite negative electrode material of a lithium ion secondary battery and a preparation method of the silicon oxide / carbon composite negative electrode material. The preparation method comprises the steps of by taking silicon oxide containing a carbon source as a raw material, preparing SiO2 and a xerogel precursor consisting of SiO and pyrolytic carbon by adopting a sol-gel method, supplementing the carbon source to perform high-energy ball milling mixing and high-temperature solid phase pyrolysis, carbonizing and partially reducing the silicon oxide, performing ball milling crushing to obtain a final composite material product, wherein the mass ratio of SiO2 to SiO in the silicon oxide / carbon composite material is (2-6):1, and the pyrolytic carbon accounts for 40-70% of the total weight of the composite material. The composite material of SiO2, SiO and the pyrolytic carbon, prepared by the preparation method disclosed by the invention, is high in capacity, long in cycle life and good in rate capability, is applied to the lithium ion secondary battery, and can significantly improve the specific energy. The preparation method disclosed by the invention is simple in equipment, easy in operation, easily-controllable in process condition and suitable for large-scale production.

Description

technical field [0001] The invention relates to a lithium ion secondary battery preparation technology, in particular to a silicon oxide / carbon composite negative electrode material for a lithium ion secondary battery and a preparation method thereof. Background technique [0002] At present, commercialized lithium-ion secondary battery anode materials mainly use carbon materials. However, the low theoretical capacity of such materials, high irreversible capacity in the first week, and poor safety during overcharging make it difficult for carbon materials to meet the requirements of high-energy power supplies. [0003] Silicon is considered to be one of the most competitive candidate anode materials for next-generation lithium-ion secondary batteries due to its high theoretical capacity, abundant resources, and discharge potential close to that of lithium or graphite. However, silicon has a short cycle life due to its large volume expansion rate and poor electrical conducti...

Claims

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Application Information

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IPC IPC(8): H01M4/36
CPCH01M4/36H01M4/483H01M4/625H01M10/0525Y02E60/10
Inventor 杨化滨时晶刘方
Owner NANKAI UNIV
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