Method for preparing porous silicon carbon nanotube composite negative electrode material of lithium ion battery by diatomite

A technology of carbon nanotube composite and silicon-carbon composite materials, which is applied in the direction of battery electrodes, secondary batteries, circuits, etc., can solve the problems of poor cycle stability of composite materials, high price of porous silicon materials, complicated preparation process, etc. Clear, low price, and simple preparation process conditions

Inactive Publication Date: 2016-08-10
NORTHEAST DIANLI UNIVERSITY
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Problems solved by technology

[0003] Chinese Invention Patent Publication (Announcement) No. CN102208636A discloses a porous silicon-carbon composite material prepared from diatomite and its application. The preparation method is to reduce diatomite to obtain silicon with a porous structure by using a metal thermal reduction method. The precursors of porous silicon and carbon are dissolved in the corresponding solvents, and the dispersed mixed solution is carbonized under a protective atmosphere to prepare coated porous silicon / carbon composites, but this type of coated silicon-carbon composites are used with lithium ions During the preparation of the negative electrode of the battery, the carbon layer is easily broken during the cycle, resulting in poor cycle stability of the composite material. The first cycle can only reach 1500mAh / g, and no more cycles
[0004] China Invention Patent Publication (Notice) No. CN102185128A discloses a silicon-carbon composite material, which uses porous silicon as a substrate to directly grow one-dimensional carbon nanomaterials on its surface, and wraps the one-dimensional carbon nanomaterials and porous silicon substrates. Covered with amorphous carbon, the composite material is applied to the preparation of lithium-ion battery anode materials, and has stable cycle performance. The constant current charge and discharge test is carried out at a current density of 300mA / g, and the composite material shows the first time of 1149mAh / g. Reversible capacity, after 100 cycles, the reversible capacity is 10871149mAh / g, and the capacity retention rate is as high as 95%. However, there are disadvantages such as high price of porous silicon materials used as raw materials, complicated preparation process, and low production efficiency.

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  • Method for preparing porous silicon carbon nanotube composite negative electrode material of lithium ion battery by diatomite
  • Method for preparing porous silicon carbon nanotube composite negative electrode material of lithium ion battery by diatomite
  • Method for preparing porous silicon carbon nanotube composite negative electrode material of lithium ion battery by diatomite

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Embodiment 1

[0034] Example 1 A kind of diatomite of embodiment 1 prepares the method for lithium-ion battery porous silicon carbon nanotube composite negative electrode material, prepares according to the following steps:

[0035] Grind natural diatomaceous earth and dissolve it in 0.01M sodium hydroxide aqueous solution, then filter and dry the suspension and collect it. Subsequently, diatomite is roasted in the air at 600°C for 2 hours to remove organic matter, and then poured into 95°C , 6M sulfuric acid solution to remove impurities such as iron oxide, aluminum oxide, magnesium oxide and calcium oxide. Finally, the purified diatomite is filtered, washed, and then dried to obtain purified diatomite. Mix the purified diatomaceous earth and magnesium powder at a mass ratio of 1:1, then place the homogeneously mixed sample in a muffle furnace, and bake it at 700°C for 3 hours in an argon atmosphere, until the temperature in the muffle furnace is naturally Take it out after cooling to ...

Embodiment 2

[0039] Example 2 A kind of diatomite of embodiment 2 prepares the method for lithium-ion battery porous silicon carbon nanotube composite negative electrode material, prepares according to the following steps:

[0040] Natural diatomaceous earth was ground and dissolved in 0.01M aqueous sodium hydroxide solution, and then the suspension was collected by filtration and drying. Subsequently, the diatomite was roasted in the air at 600°C for 2 hours to remove organic matter, and then poured into 95°C, 6M sulfuric acid solution to remove impurities such as iron oxide, aluminum oxide, magnesium oxide and calcium oxide. Finally, the purified diatomite is filtered, washed, and then dried to obtain purified diatomite. Mix purified diatomaceous earth and magnesium powder at a mass ratio of 1:1, then place the uniformly mixed sample in a muffle furnace, and bake it at 650°C in an argon atmosphere for 5 hours, and wait for the temperature in the muffle furnace to cool naturally Take ...

Embodiment 3

[0044] Example 3 A kind of diatomite of embodiment 3 prepares the method for lithium-ion battery porous silicon carbon nanotube composite negative electrode material, prepares according to the following steps:

[0045] Natural diatomaceous earth was ground and dissolved in 0.01M aqueous sodium hydroxide solution, and then the suspension was collected by filtration and dried. Subsequently, the diatomite was roasted in the air at 600°C for 2 hours to remove organic matter, and then poured into 95°C, 6M sulfuric acid solution to remove impurities such as iron oxide, aluminum oxide, magnesium oxide and calcium oxide. Finally, the purified diatomite is filtered, washed, and then dried to obtain purified diatomite. Mix the purified diatomaceous earth and magnesium powder at a mass ratio of 1.5:1, then place the homogeneously mixed sample in a muffle furnace, and bake it at 700°C for 3 hours in an argon atmosphere, until the temperature in the muffle furnace is naturally After co...

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Abstract

The invention relates to a method for preparing a porous silicon carbon nanotube composite negative electrode material of a lithium ion battery by diatomite. The method is characterized in that the diatomite is a silicon source, comprises the steps of preparing porous silicon, preparing a porous silicon matrix surface supported catalyst precursor and preparing a porous silicon carbon nanotube composite material, has the advantages of availability in raw material, low cost, clearness in morphology of the prepared porous silicon, high capacity of the silicon carbon composite material, cycle stability, high production efficiency, low cost and the like, and is suitable for industrial production. Under the test in which current density is 100mA / g, the initial reversible specific capacity of a negative electrode, prepared from the material, of the lithium ion battery reaches 1,529.1mAh / g, the reversible specific capacity reaches 885.4mAh / g after circulation of 40 times, and the subsequent cycle capacity is almost unchanged; and through the rate performance test, the reversible specific capacity is restored to about 800mAh / g when the current density is restored to 100mA / g, and the test shows that the material is high in connection tightness performance.

Description

technical field [0001] The invention belongs to the field of negative electrode materials for lithium ion batteries, in particular to a method for preparing porous silicon carbon nanotube composite negative electrode materials for lithium ion batteries from diatomite. Background technique [0002] The lithium storage capacity of negative electrode materials is a key factor restricting the application range of lithium-ion batteries. The theoretical specific capacity of current commercialized graphite-based carbon negative electrode materials is only about 372mAh / g, and the theoretical lithium storage capacity of silicon is as high as 4200mAh / g. The lithium intercalation platform is slightly higher than that of graphite, and the safety hazard is small. It shows a volume change of up to 300%, which leads to the pulverization of material particles, the destruction of the conductive network inside the electrode, and the poor conductivity. Therefore, the above-mentioned shortcomin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/38H01M4/62H01M4/1395H01M10/0525
CPCH01M4/1395H01M4/366H01M4/386H01M4/625H01M10/0525H01M2004/021Y02E60/10
Inventor 张瑛洁崔学军姜永久刘洪兵
Owner NORTHEAST DIANLI UNIVERSITY
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