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Preparation method of silicon composite anode material provided with gradient change coating layer on surface

A gradient change, negative electrode material technology, applied in battery electrodes, electrical components, circuits, etc., can solve problems such as capacity fading, poor solvent compatibility, peeling, etc.

Active Publication Date: 2014-04-02
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In terms of negative electrode materials, the current commercial lithium-ion batteries mainly use graphite-based carbon negative electrode materials, which mainly have the following problems: the theoretical specific capacity of graphite is 372mAh / g; It is easy to precipitate "lithium dendrites" and cause safety hazards; solvent compatibility is poor, and it is easy to peel off in low-temperature electrolytes such as propylene carbonate, resulting in capacity decay
[0005] There are many studies on the modification of porous silicon, but there is no research on the use of chemical vapor deposition to deposit a tight coating layer on the surface of porous silicon with a gradient change from Si to SiC and then to C.

Method used

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  • Preparation method of silicon composite anode material provided with gradient change coating layer on surface
  • Preparation method of silicon composite anode material provided with gradient change coating layer on surface
  • Preparation method of silicon composite anode material provided with gradient change coating layer on surface

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 1) Weigh magnesium powder and mesoporous silica according to the molar ratio Mg:Si=2:1, and perform ball milling and mixing treatment in a ball mill. The obtained precursor is placed in an atmosphere protection furnace at 650 degrees for 5 hours. The atmosphere condition is an argon-hydrogen mixed gas containing 5% hydrogen by volume, and the heating rate is 2°C / min.

[0020] 2) The obtained powder material was added to 1M hydrochloric acid solution and stirred for 10 hours, washed repeatedly with deionized water and ethanol, and then vacuum-dried at 80 degrees for 10 hours.

[0021] 3) The powder obtained in step 2) is placed in a multi-stage vapor deposition reaction furnace for vapor deposition coating treatment. Such as figure 1 As shown, the holding section of the multi-stage vapor deposition reaction furnace has 11 independently controllable furnaces, and the atmosphere condition is a mixture of nitrogen, monosilane and methane. Monosilane and methane are vapor ...

Embodiment 2

[0025] 1) Weigh magnesium powder and mesoporous silica according to the molar ratio Mg:Si=3:1, and perform ball milling and mixing treatment in a ball mill. The obtained precursor is placed in an atmosphere protection furnace at 700 degrees for 4 hours. The atmosphere condition is an argon-hydrogen mixed gas containing 5% hydrogen by volume, and the heating rate is 6°C / min.

[0026] 2) The obtained powder material was added to 1M hydrochloric acid solution and stirred for 10 hours, washed repeatedly with deionized water and ethanol, and then vacuum-dried at 80 degrees for 10 hours.

[0027] 3) The powder obtained in step 2) is placed in a multi-stage vapor deposition reaction furnace for vapor deposition coating treatment. The holding section of the multi-stage vapor deposition reaction furnace has 5 independently controllable furnaces, and the atmosphere condition is a mixed gas of argon, disilane and ethane. Disilane and ethane are vapor deposition gases, and their total vo...

Embodiment 3

[0031] 1) Weigh magnesium powder and mesoporous silica according to the molar ratio Mg:Si=4:1, and perform ball milling and mixing treatment in a ball mill. The obtained precursor is placed in an atmosphere protection furnace at 750 degrees for 3 hours. The atmosphere condition is an argon-hydrogen mixed gas containing 5% hydrogen by volume, and the heating rate is 8°C / min.

[0032] 2) The obtained powder material was added to 1M hydrochloric acid solution and stirred for 10 hours, washed repeatedly with deionized water and ethanol, and then vacuum-dried at 80 degrees for 10 hours.

[0033] 3) The powder obtained in step 2) is placed in a multi-stage vapor deposition reaction furnace for vapor deposition coating treatment. The holding section of the multi-stage vapor deposition reaction furnace has three independently controllable furnaces, and the atmosphere condition is a mixed gas of helium, silicon tetrafluoride and acetylene. Silicon tetrafluoride and acetylene are vapor...

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Abstract

The invention discloses a preparation method of a silicon composite anode material provided with a gradient change coating layer on the surface, and aims to overcome conventional modification defects of a silicon anode material. According to the preparation method, a porous silicon material is prepared firstly, and on the basis, a chemical vapor deposition method is adopted to uniformly deposit a coating layer on the surface of the porous silicon material, wherein the coating layer adopts an elemental Si-SiC-C transition structure. A test is performed in a vapor deposition reacting furnace provide with segmented temperatures, independently controllable atmosphere and a plurality of furnace chambers. Compared with the prior art, a gradient change process is achieved through the surface coating layer, an obvious interface structure is not formed, the coating layer is tight, so that a volume effect and electric conductivity of the silicon-based anode material in a battery charge-discharge process are inhibited effectively, and the cycling stability of the material is improved greatly. The preparation method is simple in technology and suitable for large-scale industrial production, and has wide application prospect in the field of lithium ion batteries.

Description

technical field [0001] The invention relates to the fields of preparation of electrochemical materials and new energy sources, in particular to a method for preparing a silicon composite negative electrode material with a gradient coating layer on the surface. Background technique [0002] Traditional energy materials such as coal and petroleum are increasingly in short supply around the world, and people are looking for new renewable resources. Lithium-ion battery because of its high voltage. It is popular for its advantages of high capacity density, no memory effect, long life, green and pollution-free. With the development of green energy technology and low-carbon economy, the market has put forward higher requirements for the next generation of lithium-ion batteries: high energy density, high safety, and long cycle life. In terms of negative electrode materials, the current commercial lithium-ion batteries mainly use graphite-based carbon negative electrode materials, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36
CPCH01M4/386H01M4/625H01M4/628Y02E60/10
Inventor 杨茂萍郭钰静
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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