Preparation method of silicon/carbon multi-component composite negative electrode material

A negative electrode material and multi-component composite technology, which is applied in the field of preparation of a silicon/carbon multi-component composite negative electrode material for lithium-ion batteries, can solve the problems of low material density, easy to agglomerate, and difficult to disperse, and achieve the effect of firm combination

Active Publication Date: 2014-01-29
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
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Problems solved by technology

[0004] However, in the prior art of preparing silicon-based composite negative electrode materials, the preparation process is pron

Method used

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  • Preparation method of silicon/carbon multi-component composite negative electrode material

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Embodiment 1

[0036] (1) Surface modification treatment of carbon nanotubes: first put carbon nanotubes into a mixed acid of concentrated sulfuric acid and concentrated nitric acid (volume ratio 7:1) to heat and reflux, filter and dry to obtain carboxylated carbon nanotubes .

[0037] (2) Surface modification of nano-silicon: first, heat nano-silicon (1g) in the air (400°C) to properly oxidize the surface to form a layer of silicon oxide, and then use 3-aminopropyltriethyl 1ml of oxysilane was used to aminate the above-mentioned slightly oxidized nano-silicon under the condition of heating to reflux in toluene (15ml).

[0038] (3) Preparation of primary silicon-carbon nanotube / amorphous carbon composite negative electrode material: the carboxylated carbon nanotubes obtained in step (1) and the aminated nano-silicon (carboxylated carbon nanotubes accounted for Spray drying-55% of the weight of the pyrolysis material, silicon amide accounts for 35% of the weight of the spray drying-pyrolysis...

Embodiment 2

[0043] (1) Surface modification of carbon nanotubes: first put carbon nanotubes into a mixed acid of concentrated sulfuric acid and concentrated nitric acid (volume ratio 3:1) to heat and reflux, filter and dry to obtain carboxylated carbon nanotubes .

[0044] (2) Surface modification treatment of nano-silicon: firstly, nano-silicon (1g) is properly heated (500°C) in air to oxidize its surface properly to form a layer of silicon oxide. The slightly oxidized nano silicon was then aminated with ethyl silicate (1ml) under the condition of heating to reflux with toluene (15ml).

[0045] (3) Preparation of primary silicon-carbon nanotube / amorphous carbon composite negative electrode material: the carboxylated carbon nanotubes obtained in step (1) and the aminated nano-silicon (carboxylated carbon nanotubes accounted for 35% of the weight of the material after sintering, and silicon amide accounts for 45% of the weight of the material after sintering) into the tetrahydrofuran solu...

Embodiment 3

[0050] (1) Surface modification of carbon nanotubes: first put carbon nanotubes into a mixed acid of concentrated sulfuric acid and concentrated nitric acid (volume ratio 1:1) to heat and reflux, filter and dry to obtain carboxylated carbon nanotubes .

[0051] The carbon nanotubes (10mg) obtained above were reacted with ethylenediamine (15ml) at 120°C for 24h under reflux with condensing agent dicyclohexylcarbodiimide (0.1g) to form the amide bonds and form amino groups on carbon nanotubes to obtain aminated carbon nanotubes.

[0052] (2) Surface modification treatment of nano-silicon: firstly, nano-silicon is properly heated to 600°C in the air to oxidize its surface properly to form a layer of silicon oxide.

[0053] (3) Preparation of a silicon-carbon nanotube / amorphous carbon composite negative electrode material: the aminated carbon nanotubes obtained in step (1) and the slightly oxidized nano-silicon (aminated carbon nanotubes) obtained in step (2) Accounting for 50% ...

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Abstract

The invention provides a preparation method of a silicon/carbon multi-component composite negative electrode material. The preparation method comprises the following steps: (1) preparing a carboxyl carbon nano-tube by using acid and a carbon nano-tube, or preparing an aminated carbon nano-tube by using the carboxyl carbon nano-tube; (2) oxidizing the surface of nanometer silicon so as to generate a layer of silicon oxide, or aminating slightly oxidized nanometer silicon by using ammonia-containing organosilane under the condition of heating reflux; (3) adding the carboxyl carbon nano-tube and the aminated nanometer silicon, or the carboxyl carbon nano-tube and the slightly oxidized nanometer silicon to an organic carbon source-containing solvent, dispersing and carrying out spray drying-pyrolysis; (4) mixing a material obtained in the step (3) with asphalt, and sequentially carrying out low-temperature, constant temperature and high-temperature heat treatments, thus obtaining a secondary silicon-carbon nano-tube/amorphous carbon composite negative electrode material; and (5) carrying out airflow crushing, grading, adding to the organic carbon source-containing solvent, carrying out spray drying-pyrolysis or spray pyrolysis, and carrying out high-temperature treatment, thus obtaining the silicon/carbon multi-component composite negative electrode material. The silicon/carbon multi-component composite negative electrode material prepared by the method has the advantages of large reversible capacity, designable capacity, good cycle performance, high tap density and the like.

Description

technical field [0001] The invention belongs to the field of preparation of lithium ion battery materials, and relates to a preparation method of a silicon / carbon multi-element composite negative electrode material for lithium ion batteries. Background technique [0002] Lithium-ion batteries are widely used in various portable electronic devices and electric vehicles due to their advantages such as large specific energy, high working voltage, low self-discharge rate, small size, and light weight. The current commercial lithium-ion battery anode material is mainly graphite, but its theoretical capacity is only 372mAh g -1 , high rate charge and discharge capacity is low, poor low temperature performance and other reasons, can no longer meet the demand for high energy density power supply in the field of lithium ion battery applications. Therefore, there is an urgent need to develop a new type of anode material for lithium-ion batteries with high specific capacity. [0003]...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/38H01M4/583B82Y30/00
CPCB82Y40/00H01M4/583Y02E60/10
Inventor 郭华军孟奎苏明如李新海王志兴彭文杰胡启阳
Owner CENT SOUTH UNIV
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